Category: 20850-43-5

Related Products of 20850-43-5, 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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows.

Taking 10 g about 89.7% content piperazine pyrimidine, 12 g triethylamine, 34 ml isopropanol into 100 ml three port into reaction, stirring at the room temperature under the chlorosilane dropping pepper, in 30 minutes in the transfusion. Heating to 50 C, thermal insulation 4 hours, stirring under cooling to room temperature, filter, recovery mother liquor, in the filter cake by adding 20 ml water beating, filtering, adding 10 ml water washes filters cake. 50 C drying, the crude product shall piribedil 16.6 g, HPLC analysis content 99.2%. Yield 92%

The chemical industry reduces the impact on the environment during synthesis 5-(Chloromethyl)benzo[d][1,3]dioxole. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Taicang Hongshan Environmental Protection Technology Co., Ltd.; Liu Lu; (9 pag.)CN107216318; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 20850-43-5, 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. 20850-43-5 name is 5-(Chloromethyl)benzo[d][1,3]dioxole, 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.

ake 10g about 89.7% content of piperazine pyrimidine, 12g triethylamine, 34ml isopropanol into 100ml three reaction flask, dropping peppermint chloride at room temperature under stirring, dropping over 30 minutes. Heated to 50 , incubated for 2 hours, cooled to room temperature with stirring, filtered, the mother liquor was recovered, the filter cake was added 20ml water beating, suction filtration, plus 10ml water washing cake. 50 drying, get piribedil crude 16.6g, HPLC analysis content of 99.2%. Yield 92%; 16g of crude piribedil (99.2%), 0.3g of activated charcoal and 42ml of absolute ethanol were added into a 100ml single-necked flask and heated to the reflux temperature for 0.5 hour. The activated carbon was removed by hot filtration and the filtrate was cooled and crystallized under stirring to obtain a white Crystalline solid. Filtered, rinsed with a small amount of anhydrous ethanol, and dried to obtain 14.76g of the first crystal product of piribedil, the content of which was 99.90% by HPLC and the refined yield was 90.33%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-(Chloromethyl)benzo[d][1,3]dioxole, and friends who are interested can also refer to it.

Reference:
Patent; Taicang Datang Chemical Fiber Factory; Liu Huifeng; (9 pag.)CN107266429; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-(Chloromethyl)benzo[d][1,3]dioxole

To a slurry of magnesium turnings (1.09 g, 44.8 mmol) in 5 mL of THF was added iodine (0.0650 g, 0.256 mmol), followed by a solution of 5-(chloromethyl)benzo[d][l,3]dioxole. (6.55 g, 38.4 mmol) in 30 mL of THF. After 1 minute, the exothermic reaction mixture was placed in an ice bath for 1 minute and then stirred at ambient temperature for 1 hour. TMEDA (7.68 ml, 51.2 mmol) was added to the reaction and the mixture was cooled to -78 0C for 5 minutes at which point a solution of (E)-N-((S)-2,3-bis(tert- butyldimethylsilyloxy)propylidene)-2-methylpropane-2-sulfinamide (5400 mg, 12.8 mmol) in 25 mL THF was added via a syring pump over 15 minutes. The reaction was allowed to warm to RT over the course of 2 hours then stirerd at RT for an additional hour. The mixture was diluted with ethyl acetate (10O mL) and poured in saturated ammonium chloride (250 mL). The aqueous layer was extracted with ethyl acetate (2 x 250 mL) and the combined organic layers were washed with water and then brine and dried over Na2Stheta4. The organic colvents were filtered, concentrated under reduced pressure and the crude material was purified by silica gel to provide N-((2R,3 S)-I- (benzo[d][l,3]dioxol-5-yl)-3,4-bis(tert-butyldimethylsilyloxy)butan-2-yl)-2- methylpropane-2-sulfinamide (4.51 g, 63.1% yield) as a colorless oil.

According to the analysis of related databases, 20850-43-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AMGEN INC.; WO2008/147547; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 20850-43-5, A common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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.

Step 7:Preparation of compound Ig: 2-(Benzo[l,3]dioxol-5-ylmethyl-methyl-amino)-ethanol.2-(Methylamino)ethanol (22.0 g, 290 mmol) was added to a stirred solution of 3,4- methylenedioxybenzyl chloride (25.0 g, 147 mmol) in DCM (45 mL) at -780C under nitrogen. The solution was stirred for 15 minutes at -780C then warmed to room temperature and stirred for 16h. 1.2 M NaOH (100 mL) was added and the phases were separated. The organic layer was washed water (2 x 150 mL) and concentrated under vacuum to give 25.3 g (83%) of 2-(benzo[l,3]dioxol-5-ylmethyl- methyl-amino)-ethanol as a clear oil.

The synthetic route of 20850-43-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KALYPSYS, INC.; WO2007/62417; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 20850-43-5,Some common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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.

50 g of 2-piperazin-1-ylpyrimidine, 60 g of triethylamine and 170 ml of isopropyl alcohol were put into a 100 ml three-necked reaction flask, and 58 g of piperonyl chloride was added dropwise with stirring at room temperature, and the mixture was dropped in 30 minutes, heated to 50 C, stirring to cool to room temperature, filtration, recovery of mother liquor, filter cake by adding 100ml water beating, pumping, plus 50ml water washing cake. Dried at 50 C, 71.5 g of piribedil crude and 99.1% by HPLC. Yield 92%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-(Chloromethyl)benzo[d][1,3]dioxole, its application will become more common.

Reference:
Patent; Suzhou Hongsen Pharmaceutical Co., Ltd.; Di, Jinxing; Fan, Chao; Lu, Hongbin; (6 pag.)CN106432212; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 20850-43-5,Some common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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 slurry of magnesium turnings (1.09 g, 44.8 mmol) in 5 mL of THF was added iodine (0.0650 g, 0.256 mmol), followed by a solution of 5-(chloromethyl)benzo[d][l,3]dioxole (6.55 g, 38.4 mmol) in 30 mL of THF. After 1 minute, the exothermic reaction mixture was placed in an ice bath for 1 minute and then stirred at ambient temperature for 1 hour. TMEDA (7.68 ml, 51.2 mmol) was added to the reaction and the mixture was cooled to -78 0C for 5 minutes at which point a solution of (E)-N-((S)-2,3-bis(tert- butyldimethylsilyloxy)propylidene)-2-methylpropane-2-sulfinamide (5400 mg, 12.8 mmol) in 25 mL THF was added via a syring pump over 15 minutes. The reaction was allowed to warm to RT over the course of 2 hours then stirerd at RT for an additional hour. The mixture was diluted with ethyl acetate (100 mL) and poured in saturated ammonium chloride (250 mL). The aqueous layer was extracted with ethyl acetate (2 x 250 mL) and the combined organic layers were washed with water and then brine and dried over Na2SO4. The organic colvents were filtered, concentrated under reduced pressure and the crude material was purified by silica gel to provide N-((2R,3S)-1- (benzo[d][l,3]dioxol-5-yl)-3,4-bis(tert-butyldimethylsilyloxy)butan-2-yl)-2- methylpropane-2-sulfinamide (4.51 g, 63.1% yield) as a colorless oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-(Chloromethyl)benzo[d][1,3]dioxole, its application will become more common.

Reference:
Patent; AMGEN INC.; WO2009/64418; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 20850-43-5, 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 20850-43-5 as follows.

Preparation of 1, 3-benzodioxol-5-ylmetlyl ethyl sulfone 8.6 g of 5-(chloromethyl)-1, 3-benzodioxol was dissolved in 20 ml of anhydrous tetrahydrofuran and 20 ml of diethyl ether and then added to magnesium at 0C. The reaction was done for 10 minutes and then for 1 hour at 50C. The reaction mixture was cooled to 0C and then slowly added to the flask containing [1,3-bis (diphenylphosphino) propane] nickel (II) dichloride as a catalyst. After the addition of 3.7 ml ethane sulfonyl chloride, the mixture was reacted for 30 minutes. The reactant was then heated to 50C and reacted for 1 hour. Then, its pH was adjusted to 7 with dilute hydrochloric acid. The resulting mixture was extracted with diethyl ether and distilled water, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was fractionated by column chromatography using ethyl acetate: n-hexane (1: 3), to give 0.3 g of the title compound of the following formula lb (Rf: 0.35, Yield: 3%). [Chemical Formula 1b] The compound was dissolved in CDC13 and TMS and then characterized by’H NMR spectroscopy. The result is as follows; ‘H NMR 5 : 1.57-1. 64 (t, 3H, J=7.3Hz), 2.78 (s, 2H), 3.60-3. 78 (q, 2H, J=7.3Hz), 5.90 (s, 2H), 6.56-6. 79 (m, 3H).

According to the analysis of related databases, 20850-43-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HAN, Sang Min; LEE, Myung Hee; CHOI, Won Chul; WO2005/70915; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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. category: chlorides-buliding-blocks

Step 2. Synthesis of 3-(benzo[d][1 ,3]dioxol-5-ylmethyl)-5-(3-nitrobenzylidene)imidazo- lidine-2,4-dione; DBU (3.82 mmol, 0.961 g) is added into solution of 5-(3-nitrobenzylidene)imidazolidine-2,4- dione (3.19 mmol, 0.743 g) at O’O and the solution left to warm to room temperature. 5- (Chloromethyl)benzo[d][1 ,3]dioxole (6.37 mmol, 2.174 g, 50% soln in CH2CI2) is added and the reaction mixture stirred for 3 hours. Subsequently 0.5 M HCL solution is added and extracted with ethylacetate (2 x 50 ml_) dried over MgSO4 and the solvent removed under reduced pressure. The obtained product is recrystallized from diisopropylether to afford 0.13 (1 1%) of 3-(benzo[d][1 ,3]dioxol-5-ylmethyl)-5-(3-nitrobenzylidene)imidazo-lidine-2,4-dione.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 20850-43-5, its application will become more common.

Reference:
Patent; LEK PHARMACEUTICAL D.D.; WO2008/43733; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 20850-43-5, 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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[[00244]] To a solution of [4- (8-AZA-BICYCLO] [3.2. [1] OCT-3-] ylamino)-6-chloro-1-(2, 2, [2-TRIFLUORO-ETHYL)-LH-QUINAZOLIN-2-] one (149 mg, 0.320 mmol) in DMF (10 mL) was added triethylamine (0.3 mL) and 5-Chloromethyl-benzo [1, 3] dioxole [(0.] 061 mL, 0.480 mmol). The solution was heated to 50 C and stirred for 6 hrs. The reaction was partitioned between ethyl acetate and water and the organic phase was washed an additional 2 x with water and brine, dried over [NA2SO4,] filtered, and concentrated. The crude residue was purified by flash chromatography (gradient elution: [0-20%] MeOH/dichloromethane) to provide 99 mg white solid [(60%). 1H] NMR (300 MHz, CDCl3) 8 ppm 2.10 (m, 4 H), 2.32 (m, 2 H), 3.56 (m, 3 H), 3.77 (s, 2 H), 4.87 (m, 2 H), 5.96 (s, 2 H), 6.77 (d, J = 8.0 Hz, [1] H), 6.83 (m, [1] H), 6.95 (d, J = 8.1 Hz, [1] H), 7.17 (m, 2 H), 7.56 (dd, J = 2.3, 8.9 Hz, [1] H), 7.91 (s, [1] H); MS (ESI [+Q1MS)] m/z 522 [[M+2H] +]

The synthetic route of 5-(Chloromethyl)benzo[d][1,3]dioxole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MILLENNIUM PHARMACEUTICALS, INC.; WO2003/106452; (2003); A2;,
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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 5-(Chloromethyl)benzo[d][1,3]dioxole

General procedure: To a mixture of 7 (0.30g, 1mmol) in DMF (6mL) was added potassium carbonate (0.83g, 6.0mmol), potassium iodide (0.01g, 0.06mmol), and (chloromethyl)cyclopropane (9a, 0.28mL, 3.0mmol) at room temperature. The mixture was stirred for 48h, poured into brine, then extracted with CH2Cl2. The organic layer was separated, dried over MgSO4, and concentrated. The crude residue was purified by silica gel column chromatography to give 10a (100mg, 28%) as a yellow oil.

The synthetic route of 20850-43-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liao, Yung-Feng; Tang, Yu-Cheng; Chang, Ming-Yun; Wang, Bo-Jeng; Hu, Ming-Kuan; European Journal of Medicinal Chemistry; vol. 79; (2014); p. 143 – 151;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics