Category: 29671-92-9

Some common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, molecular formula is CH4Cl2N2, 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. SDS of cas: 29671-92-9

2-Amino-5-chloro-3,9-dihydro-4H-pyrimido[4,5-b]indol-4-one (8) 1 g methyl sulfone was heated to melting. 7 (106.22 mg, 1.37 mmol) was added and the resulting mixture was stirred and heated at 110-120 C. to dissolve completely. 5 (200 mg, 0.837 mmol) was added in one part to the reaction mixture. Stirring was continued for 30 minutes. About 10 mL water was added to quench the reaction. Ammonia water was added to neutralize the reaction mixture. Solid precipitated out. This solid was filtered. Obtained solid was dissolved in chloroform and methanol, dried (using Na2SO4) and recrystallized.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 29671-92-9, its application will become more common.

Reference:
Patent; Gangjee, Aleem; US2009/62318; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 29671-92-9,Some common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, molecular formula is CH4Cl2N2, 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.

Method A: 2,4-diamino-6-chloropyrido[3,2-c/]pyrimidine (7.5 g, 38 mmole), e.g. prepared according to Colbry et a/. J. Heterocycl, Chem. (1984) 21 :1521 , was suspended in 6 N HCI (300 ml) and the mixture was refluxed for 5 hours. After cooling, the pH was made alkaline (pH about 9 – 10) by means of 10 N NaOH. The precipitate obtained was filtered, washed with H2O and dried at 100 0C, resulting in the pure title compound (7.0 g, yield 95 %) which was characterized by its mass spectrum as follows: MS (m/z): 197 ([M+H]+, 100).Method B: A mixture of 3-amino-6-chloro-pyridine-2-carboxamide (5.1 g, 30 mmol), chloroform-amidine hydrochloride (6.99 g, 60 mmol), dimethylsulfone (24 g) and sulfolane (2.4 ml) was heated at 165 0C for 30 min. To the hot mixture was added water (50 ml). After cooling to room temperature, a diluted ammonium hydroxide solution was slowly added drop wise till pH 7. The resulting precipitate was filtered off, washed with water and dried overnight at 100 0C to give the pure title compound (5.8 g, 98 %). The obtained compound was used as such for further reactions without additional purification. M. p. >330C; elemental analysis calc. for C7H5CIN4O (196.6): C 42.77 H 2.56 N 28.50. Found: C 41.61 H 2.74 N 28.76.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Carbamimidic chloride hydrochloride, its application will become more common.

Reference:
Patent; 4 AZA Bioscience nv; WO2006/135993; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 29671-92-9, These common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, its 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.

2-Amino-6-(4-metho e Experimental procedure taken from Abdillahi et al. [17], Savall ef a/.[18] and Edwards et al. [19]. Ethyl 3-amino-5-(4-methoxyphenyl)thiophene-2-carboxylate (0.832 g, 3.00 mmol) and chloroformamidine hydrochloride (0.517 mg, 4.50 mmol) were mixed with dimethylsulfone (0.847 g, 9.00 mmol) and heated at 140-150 C for one hour. Subsequently, the viscous solution was cooled to room temperature and mixed with an aqueous ice-cooled solution of sodium hydroxide (0.400 g, 10.0 mL). The aqueous solution was extracted with ethyl acetate (3 x 25 mL). The aqueous solution was neutralized with diluted hydrochloric acid (5% v/v) until precipitation started. The precipitates were filtered of and recrystallized from ethanol to yield brown powder (Yield: 36.0%). Mp = 326-328 C. 1H-NMR (DMSO-d6, 400 MHz): 3.81 (s, 3H, CH3), 6.90 (s, 2H, NH2), 7.01 -7.04 (m, 2H, ArH), 7.25 (s, 1 H, ArH), 7.68-7.71 (m, 2H, ArH). 3C-NMR (DMSO-de, 100 MHz): 56.1 (prim. C); 1 4.6 (2C), 1 18.3, 127.4 (2C) (tert. C); 1 10.5, 125.8, 149.7, 155.5, 158.9, 160.1 , 174.4 (quart. C).

Statistics shows that Carbamimidic chloride hydrochloride is playing an increasingly important role. we look forward to future research findings about 29671-92-9.

Reference:
Patent; KTB TUMORFORSCHUNGSGESELLSCHAFT MBH; KUBBUTAT, Michael; SCHAeCHTELE, Christoph; EHLERT, Jan; TOTZKE, Frank; KUNICK, Conrad; WOeLFEL, Sebastian; WEBER, Holger; WO2014/79545; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 29671-92-9,Some common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, molecular formula is CH4Cl2N2, 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.

Example 7 Synthesis of 2-amino-8-chloro-3H-benzo[4,5]furo[3,2-d]pyrimidin-4-one; To a solution of S-amino-S-chlorobenzofuran-l-carboxylic acid methyl ester (5.0 g, 22.16 mmol, 1 eq) in sulfolane (25 ml) is added chloroformamidine hydrochloride (3.82 g, 33.24 mmol, 4.5 eq) at 100 0C and the reaction mixture is stirred further at 160 0C for an hour, it is cooled down to 50 0C and diluted with methanol (75 ml), the precipitated product is filtered off, dried in vacuo at 80 0C. A yellowish solid (3.85 g, 16.34 mmol, 73.73%) is obtained.1H NMR (DMSO-de): 7.67 (dd, IH), 7.82 (d, IH), 8.06 (d, IH)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Carbamimidic chloride hydrochloride, its application will become more common.

Reference:
Patent; CELLZOME (UK) LTD.; WO2008/62013; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 29671-92-9, name is Carbamimidic chloride 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 29671-92-9, COA of Formula: CH4Cl2N2

(1) Add methyl 3-amino-5-bromopyrimidinecarboxylate (6.2 g, 27 mmol) to a 250 mL sealed tube.Chloroformamidine hydrochloride (3.4 g, 30 mmol) and dimethyl sulfone (50.8 g, 20 mmol) were heated to 140oC and stirred for 6 hours. After cooling to room temperature, 50 mL of water was added to the reaction solution, followed by ultrasonication for 30 minutes. The residue was filtered. Water, acetone washing, vacuum drying to obtain a tan solid 1 (yield = 65%),

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, Carbamimidic chloride hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tsinghua University; Liao Xuebin; He Lei; Wang Zhisong; Gao Yan; (59 pag.)CN108069963; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 29671-92-9, 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. 29671-92-9, name is Carbamimidic chloride hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

Chloroformamidine hydrochloride with Sodium hydroxide is put into A 25 mL round bottom flask was charged with 3 mL of acetonitrile solvent and pretreated Neutralize the acid, get free amidine. Then, ethyl benzoylacetate and perfluoroiodobutane were successively added at room temperature. indoor Light and room temperature for 8h, TLC monitoring reaction end, stop the reaction, the mixture. [0119] Ethyl benzoylacetate: Perfluorooiodobutane: Chloroformamidine hydrochloride: Sodium hydroxide = 1.0: 1.1: 1.1: 4.1; [0120] 2. The mixture was extracted three times with water, the organic phases were combined and the organic solvent was removed by distillation under reduced pressure to give crude product. [0121] 3. The crude product was chromatographed on silica gel eluting with eluent (petroleum ether: ethyl acetate = 30: 1 (nu: nu) A white solid was obtained as the product ethyl-2-chloro-4-perfluoropropyl-6-phenylpyrimidine-5-carboxylate in 57% yield.

The chemical industry reduces the impact on the environment during synthesis Carbamimidic chloride hydrochloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Liaoning University; Liang Fushun; Wang Rui; Han Zhengbo; Su Zhongmin; (12 pag.)CN106831603; (2017); A;,
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. 29671-92-9, name is Carbamimidic chloride hydrochloride, A new synthetic method of this compound is introduced below., COA of Formula: CH4Cl2N2

The mixture of compound 1 (50 g, 0.318 mol), compound 2 (54.86 g, 0.477 mol) and methylsulfonylmethane (150.6 g, 1.59 mol) was refluxed overnight, cooled and evaporated. The resulting residue was washed mixture EtOAc-iPrOH (1 : 2). The yield was 41.65 g (0.249 mol, 78%).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; SHY THERAPEUTICS LLC; HADARI, Yaron R.; CARTA, Luca; SCHMERTZLER, Michael; WILLIAMS, Theresa M.; REYNOLDS, Charles H.; HUTCHESON, Rebecca; (1452 pag.)WO2018/237084; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 29671-92-9, These common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, its 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.

A l l three-neck round-bottom flask equipped with a mechanical stirrer, a condenser, and a thermocouple was charged with ethyl 2-(6-amino-2,3-dichlorobenzylamino)acetate of formula (3B) (20.00 g, 72.0 mmol), chloroformamidine hydrochloride (12.44 g, 108 mmol) and acetonitrile (120 ml) under argon, and the suspension was heated to 40C. Then, acetic acid (21 ml, 363 mmol) was added and the suspension was heated to reflux (90C in oil bath). After 5 hours, the compound of formula (3B) was fully consumed as checked by HPLC. The suspension was diluted with acetonitrile (60 ml), and then N,N-diisopropylethylamine (44 ml, 252 mmol) was added drop-wise over approx. 3 minutes, and the suspension was stirred for an additional 75 minutes. Then, the reaction mixture was cooled to 50C and water (150 ml) was added. Stirring at 50C was continued for 1 hour. Then, the suspension was filtered, washed with water (30 ml), ethanol (50 ml), and methyl i-butyl ether (50 ml), and dried (23C, 100 mbar, N2 bleed, 18 hours) to give 13.48 g of anagrelide as a pale beige solid (73% of theory) in 99.53% purity (HPLC, external standard)).

Statistics shows that Carbamimidic chloride hydrochloride is playing an increasingly important role. we look forward to future research findings about 29671-92-9.

Reference:
Patent; SYNTHON BV; GIELING, Reinerus Gerardus; LINDEN van der, Johannes Bastiaan; VERKERK, Pascal Renart; MEL?A, Petr; WO2014/139572; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 29671-92-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 29671-92-9 name is Carbamimidic chloride hydrochloride, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

INTERMEDIATE 7 2-Aminothieno [3 ,4-d]pyrimidin-4-ol A mixture of methyl 4-aminothiophene-3-carboxylate (1.0 g, 6.4 mmol), chioro5 formamidine hydrochloride (1.83 g 15.9 mmol) and dimethyl sulfone (2.99 g, 31.8 mmol)was finely ground with a pestle and mortar, and the mixture was heated at 130C for 40 minutes. Water was poured into the reaction mixture, and concentrated ammonia solution was added to basify the reaction solution (ice bath). The precipitate was collected, washed with water and dried in vacuo, to provide the title compound (0.99 g, 92%) as ayellow solid. ?3C NMR (75 MHz, DMSO-d6) oe 159.7, 151.4, 148.8, 127.4, 123.7, 108.4. MS m/z (%) 168 [M+H].

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Carbamimidic chloride hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; FORD Daniel James; HUANG Qiuya; NEUSS Judi Charlotte; REUBERSON James Thomas; VANDERHOYDONCK Bart; WO2015/193168; (2015); A1;,
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. 29671-92-9, name is Carbamimidic chloride hydrochloride, A new synthetic method of this compound is introduced below., Computed Properties of CH4Cl2N2

To a suspension of Ig (400 mg, 0.66 mmol) in methanol (26 mL) was dropwise added concentrated HCl (4.5 mL) while stirring. The mixture was stirred at room temperature for 1 h. The resulting solution was concentrated in vacuo and dried. The residue was then mixed with methyl sulfone (6 g) and chloroamidine hydrochloride (113 mg, 0.99 mmol) in a microwave vial, and heated at 150 0C for 1 h. While cooling to room temperature, the mixture was treated with IN ammonium hydroxide (5 mL) and ethyl acetate (5 mL) with vigorous stirring. The organic layer was concentrated and the residue was purified by silica gel column chromatography (EtOAc / hexanes), affording 3a as an oil (0.05 g, 13%). MS = 584.0 (M+ H+). 1H NMR (300 MHz, CDCl3): B 8.09 (s, IH), 7.2-7.4 (m, 15H), 5.33 (s, IH), 4.4-4.8 (m, 7H), 3.96 (m, IH), 3.86 (m, 2H), 1.16 (s, 3H).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; GILEAD SCIENCES, INC.; BUTLER, Thomas; CHO, Aesop; KIM, Choung, U.; XU, Jie; WO2010/93608; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics