Succinylcholine Chloride synthesis
- Product Name:Succinylcholine Chloride
- CAS Number:71-27-2
- Molecular formula:C14H30Cl2N2O4
- Molecular Weight:361.3
Yield:71-27-2 83.2%
Reaction Conditions:
Stage #1:choline chloride;succinoyl dichloride with calcium chloride in ethanol;chloroform at 50 - 60; for 1 h;
Stage #2: with pyridine in ethanol;chloroform; pH=5 - 6 at 5 - 25;Concentration;Temperature;
Steps:
3; 4 Example 3
Treatment of alcohol-free chloroform: The commercially available analytical pure chloroform (containing stabilizer ethanol,Ethanol content (0.3-1.0percent) is obtained by drying and filtering with anhydrous calcium chloride overnight.Connected with condenser, drying device,Put a stir bar, choline chloride (57.24g, 0.41mol) and alcohol-free chloroform (80mL) into the reaction flask (500mL) of the lye absorption device. The temperature is raised and refluxed to azeotropically remove water. After the chloroform is evaporated to anhydrous (about 40mL of chloroform), succinyl chloride (31.00g, 0.20mol) is added dropwise at 50-60°C, and the reaction is carried out at 60°C for 1h. After the reaction solution dropped to 5°C, pyridine (32.3mL, 0.40mol) was directly added dropwise to adjust the pH to 5-6 and the temperature did not exceed 25°C, and anhydrous EtOH (160mL) was added to dissolve. After dropping to 5°C, under rapid stirring, distilled water (14.4g, 0.80mol) was added at one time and left to stand, and a large amount of crystalline white solid was precipitated. Suction filtration, washing with 95percent EtOH (80 mL×2), and suction filtration. 95percent EtOH (550mL×2) was recrystallized twice and dried to obtain 66.16 g of succinylcholine chloride, with a yield of 83.2percent and a purity of 98.89percent.
References:
Shanghai Xudonghaipu Pharmaceutical Co., Ltd.;Chinese Academy Of Sciences Shanghai Pharmaceutical Institute;Tan Changheng;Jiang Kun;Zhang Shijun;Lu Xiang;Mi Boquan CN110776435, 2020, A Location in patent:Paragraph 0063-0073
19249-04-8
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