Category: 26487-67-2

Some common heterocyclic compound, 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, molecular formula is C8H17Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. HPLC of Formula: C8H17Cl2N

Compound 4 (200mg, 0.75mmol) refluxed with K2CO3 (259.42mg, 1.87mmol), 1-(2-Chloro-ethyl)-azepane hydrochloride (148.58mg, 0.75mmol) in acetone furnished 7 (220mg, 75percent) as brown viscous oil. 1H NMR (300MHz, CDCl3): delta 7.21?7.06 (m, 8H), 6.91?6.78 (m, 3H), 6.64?6.63 (m, 1H), 5.59 (s, 1H), 4.07 (t, J=6.0, 2H), 2.97 (t, J=6.1, 2H), 2.81 (t, J=5.6, 4H), 1.69?1.61 (m, 8H); 13C NMR (CDCl3, 50MHz): delta 157.5, 148.4, 144.1, 136.2, 129.8 (2C), 128.7 (2C), 128.4 (2C), 126.6, 126.5, 126.2, 124.4, 114.4 (2C), 65.7, 57.8, 54.9 (2C), 51.3, 25.7 (3C), 24.1; IR (Neat): 3019, 2938, 2362, 1610, 1509, 1218, 763cm?1; MS (ESI): m/z 392 (M+H)+; Anal. Calcd for C25H29NOS: C, 76.68; H, 7.46; N, 3.58. Found: C, 76.72; H, 7.39; N, 3.61.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 26487-67-2, its application will become more common.

Reference:
Article; Singh, Priyanka; Manna, Sudipta Kumar; Jana, Amit Kumar; Saha, Tiash; Mishra, Pankaj; Bera, Saurav; Parai, Maloy Kumar; Srinivas Lavanya Kumar; Mondal, Sankalan; Trivedi, Priyanka; Chaturvedi, Vinita; Singh, Shyam; Sinha, Sudhir; Panda, Gautam; European Journal of Medicinal Chemistry; vol. 95; (2015); p. 357 – 368;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 1-(2-Chloroethyl)azepane hydrochloride

Example 2: Synthesis of 2-((2-(azepan-1-yl)ethoxy)methyl)pyrazolo[1 ,5-a]pyridine maleate 0.12 g (3 mmol) of a 60percent NaH suspension in mineral oil were added under nitrogen to a solution of pyrazolo[1 ,5-a]pyridin-2-ylmethanol (100 mg, 0.67 mmol) in 5 mL of dry THF. The mixture was stirred for 5 h at room temperature, and after this time, was added 1 -(2-chloroethyl)azepane hydrochloride (201 mg, 1 .01 mmol) suspended in 8 ml_ of THF with 200muIota of triethylamine (TEA). The mixture was heated at 55 5C for 18 h, allowed to cool to room temperature, quenched with water and extracted with EtOAc, and washed with water. The organic layers were dried over Na2S04 and concentrated under vacuum to afford 0.22 g (65percent) of brown oil. Maleate salt was obtained following the same procedure as for example 1 . 1 H NMR (CDCI3) delta ppm: 8.42 (d, J = 6.8 Hz, 1 H), 7.52 (d, J = 8.8 Hz, 1 H), 7.20 – 7.06 (m, 1 H), 6.78 (t, J = 6.9 Hz, 1 H), 6.49 (s, 1 H), 6.30 (s, 2H), 4.74 (s, 2H), 4.08 – 3.89 (m, 2H), 3.70 – 3.51 (m, 2H), 3.36 – 3.25 (m, 2H), 3.19 – 2.99 (m, 2H), 2.15 – 1 .92 (m, 2H), 1 .92 – 1 .72 (m, 4H), 1 .72 – 1 .54 (m, 2H).

The synthetic route of 26487-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LABORATORIOS DEL DR. ESTEVE S.A.; DIAZ FERNANDEZ, Jose Luis; CUBERES ALTISENT, Mª Rosa; WO2013/124341; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 26487-67-2, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Commercially available 5-chloro benzoxazoles or benzothiazoles(5 mmol) and K2CO3 (15 mmol) were added to 50 mL of DMF.The mixture was heated at 60 C and 1-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (6.5 mmol) was added. The mixture was maintained at 60 C under stirring for 3 h, then was cooled to room temperature, poured into water, and extracted with diethyl ether(3 50 mL). The organic layer was washed with brine, dried overan hydrous Na2SO4 and evaporated under reduced pressure to give are sidue, which was purified by flash column chromatography oversilica gel using ethyl acetate/methanol 8:2 v/v as eluent. Immediately after solvent evaporation, free bases were converted into hydrochlorides by dissolving the corresponding amine in diethyl ether and treating with a 1.25MHCl ethanol solution (pH 1e2). The precipitate was filtered off, washed with diethyl ether, and dried under nitrogen. The following compounds were obtained using this procedure:

The chemical industry reduces the impact on the environment during synthesis 1-(2-Chloroethyl)azepane hydrochloride. I believe this compound will play a more active role in future production and life.

Reference:
Article; Romeo, Giuseppe; Prezzavento, Orazio; Intagliata, Sebastiano; Pittala, Valeria; Modica, Maria N.; Marrazzo, Agostino; Turnaturi, Rita; Parenti, Carmela; Chiechio, Santina; Arena, Emanuela; Campisi, Agata; Sposito, Giovanni; Salerno, Loredana; European Journal of Medicinal Chemistry; vol. 174; (2019); p. 226 – 235;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 26487-67-2,Some common heterocyclic compound, 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, molecular formula is C8H17Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a solution of 1,1-bis(4-hydroxyphenyl)-2-hexyloct-1-ene (40.0 mg, 0.105 mmol) in DMF (1.80 mL) at 0 °C was added 55percent sodium hydride (dispersion in paraffin liquid, 36.7 mg, 0.841 mmol). The reaction mixture was stirred for 1 h at 50 °C and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (68.7 mg, 0.347 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 3 h at 50 °C, saturated aqueous ammonium chloride was added at 0 °C. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 9/1) to afford RID-F-S*24 (compound 16) (57.4 mg, 87percent) as a pale yellow oil

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(2-Chloroethyl)azepane hydrochloride, its application will become more common.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 26487-67-2, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 1,1-bis(4-hydroxyphenyl)-2-methylprop-1-ene (19.2 mg, 79.9 mumol) in DMF (0.80 mL) at 0 °C was added 60percent sodium hydride (dispersion in paraffin liquid, 25.6 mg, 0.640 mmol). The reaction mixture was stirred for 15 min at 50 °C and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (52.3 mg, 0.264 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 3 h at 50 °C, saturated aqueous ammonium chloride was added at 0 °C. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 15/1) to afford RID-F-S*9 (compound 21) (32.9 mg, 84percent) as a pale yellow oil

The chemical industry reduces the impact on the environment during synthesis 1-(2-Chloroethyl)azepane hydrochloride. I believe this compound will play a more active role in future production and life.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-(2-Chloroethyl)azepane hydrochloride

A solution of 4,5,6,7-tetrahydropyrazolo[1,5-a]pyridin-2-ol (66 mg, 0.477 mmol), potassium carbonate (264 mg, 1.91 mmol), 2-(hexamethylenimino)ethyl chloride hydrochloride (142 mg, 0.717 mmol) and Nal (catalytic amount) in 3 mL of DMF, was heated to 90 ºC under nitrogen for 18 h. The mixture was allowed to cool to room temperature and evaporated to dryness. The residue was partitioned between water and EtOAc, the organic layer washed with water, dried and concentrated under vacuum to afford a residue of 101 mg that was purified by flash chromatography on silica gel with EtOAc/MeOH eluent mixtures from 90:10 to 60: 40 with 1percent TEA to give 58 mg (46percent) of yellow oil.

The synthetic route of 26487-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Laboratorios del. Dr. Esteve, S.A.; Diaz-Fernandez,Jose-Luis; Cuberes-Altisent,Mª Rosa; EP2631236; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 26487-67-2, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 26487-67-2 as follows.

1-(2-Chloroethyl)azepane hydrochloride (514 mg, 2.59 mmol), 50percent NaOH (10.4 mL,12.97 mmol), and a catalytic amount of benzyltriethylammonium chloride were added to a solution of (2-phenylimidazo[2, 1 -b][1 ,3,4]thiadiazol-6-yl)methanol (120 mg, 0.52 mmol) in toluene (3 mL) under argon atmosphere. The resulting mixture was refluxed for 6 h. The reaction mixture was diluted with water and extracted withEtOAc. The organic extracts were dried with Na2504 and evaporated to dryness. The crude product was purified by silica gel column chromatography (EtOAc:MeOH mixtures of increasing polarity as eluent) to afford the desired product (393 mg, 67percent). The product was converted into the corresponding maleate salt by adding maleic acid (27 mg, 0.23 mmol) in acetone (0.25 mL), followed by filtration of the resulting solid and drying under vacuum.1H-NMR (DMSO-d6, 300 MHz) & 9.24 (s, 1H), 8.27 (s, 1H), 7.94 (m, 2H), 7.62 (m,3H), 6.00 (s, 2H), 4.55 (s, 2H), 3.78 (t, J= 5.1 Hz, 2H), 3.31 (m, 6H), 1.76 (m, 4H),1.59(m, 4H)ppm.ESI(+)-HRMS: 357.1746 [M+H].

According to the analysis of related databases, 26487-67-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LABORATORIOS DEL DR. ESTEVE, S.A.; ALCALDE-PAIS, Maria de las Ermitas; DIAZ-FERNANDEZ, Jose-Luis; MESQUIDA-ESTEVEZ, Maria, de les Neus; PALOMA-ROMEU, Laura; WO2014/6130; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 26487-67-2, The chemical industry reduces the impact on the environment during synthesis 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, I believe this compound will play a more active role in future production and life.

0.12 g (3 mmol) of a 60percent NaH suspension in mineral oil were added under nitrogen to a solution of pyrazolo[1,5-a]pyridin-2-ylmethanol (100 mg, 0.67 mmol) in 5 mL of dry THF. The mixture was stirred for 5 h at room temperature, and after this time, was added 1-(2-chloroethyl)azepane hydrochloride (201 mg, 1.01 mmol) suspended in 8 mL of THF with 200mul of triethylamine (TEA). The mixture was heated at 55 ºC for 18 h, allowed to cool to room temperature, quenched with water and extracted with EtOAc, and washed with water. The organic layers were dried over Na2SO4 and concentrated under vacuum to afford 0.22 g (65percent) of brown oil.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-(2-Chloroethyl)azepane hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Laboratorios del. Dr. Esteve, S.A.; Diaz-Fernandez,Jose-Luis; Cuberes-Altisent,Mª Rosa; EP2631236; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, molecular formula is C8H17Cl2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Application In Synthesis of 1-(2-Chloroethyl)azepane hydrochloride

EXAMPLE 9 To a solution of 7.5 g of 1,3-dihydro-5-(2-chlorophenyl)-7-chloro-2H-1,4-benzodiazepine-2-thione in a solvent mixture comprising 30 ml of a 10percent aqueous sodium hydroxide solution and 30 ml of methanol is added dropwise under ice cooling with stirring an aqueous solution of 7.0 g of 1-chloro-2-(perhydroazepin-1-yl)ethane hydrochloride over a period of about 10 minutes, and the resulting mixture is stirred at room temperature for 4 hours. The reaction mixture is diluted with water and extracted with ethyl acetate. The extract is rinsed with a 5percent aqueous sodium hydroxide solution, washed with water and dried. Thereafter the solvent is distilled off to obtain an oily residue of 2-(2-perhydroazepin-1-ylethylthio)-5-(2-chlorophenyl)-7-chloro-3H-1,4-benzodiazepine. The oily product thus obtained is treated, according to usual procedure, with 2.74 g of fumaric acid and recrystallized from isopropyl alcohol to obtain 9.9 g of 2-(2-perhydroazepin-1-ylethylthio)-5-(2-chlorophenyl)-7 -chloro-3H-1,4-benzodiazepine fumarate, m.p. 170°-171° C. Elementary analysis: for C23 H25 N3 SCl2.C4 H4 O4: Calculated: C: 57.65, H: 5.20, N: 7.47; Found: C: 57.76, H: 5.31, N: 7.40.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 26487-67-2, its application will become more common.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US4094870; (1978); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 26487-67-2, Recommanded Product: 26487-67-2

Example 7 1-(2-(1-Perhydroazepinyl)ethyl)-3,4-dimethyl-4-(3-(1H-1,2,3-triazol-4-yl)phenyl)piperidine A solution of 1-(2-chloroethyl)perhydroazepine hydrochloride (42 mg, 0.21 mmol) in N,N-dimethylformamide (1 mL) was treated with triethylamine (30 muL, 0.22 mmol) then transferred to a flask containing 3,4-dimethyl-4-(3-(1H-1,2,3-triazol-4-yl)phenyl)piperidine (Preparation 44, 45 mg, 0.176 mmol) in N,N-dimethylformamide (2 mL). Sodium iodide (32 mg, 0.21 mmol) and sodium hydrogencarbonate (18 mg, 0.21 mmol) were added and the resultant mixture was heated at 60°C overnight. The solvent was then removed in vacuoand the residue was partitioned between saturated aqueous sodium hydrogencarbonate solution (5 mL) and dichloromethane (5 mL). The phases were separated and the aqueous layer was further extracted with dichloromethane (2 x 5 mL). The combined extracts were dried over Na2SO4, filtered and concentratedin vacuo.The residue was purified by reversed phase preparative HPLC (condition 2) to give the acetate salt of the title compound. The free base was obtained by treating with dilute aqueous ammonia solution (2 mL) and extracting with ether (4 x 3 mL). Drying over Na2SO4, filtering andevaporation to dryness gave the title compound as a white solid (16 mg, 24percent). NMR (CDCl3, selected data for the free base): 0.8 (d, 3H), 1.35 (s, 3H), 1.6-1.8 (m, 9H), 2.10 (m, 1H), 2.4-2.5 (m, 2H), 2.6-3.0 (m, 11H), 7.25 (d, 1H), 7.35 (t, 1H), 7.55 (d, 1H), 7.85 (s, 1H), 7.95 (s, 1H). MS (thermospray): M/Z (MH+) 382.6; C23H35N5+ H requires 382.3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(2-Chloroethyl)azepane hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; PFIZER INC.; Pfizer Limited; EP1072601; (2001); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics