1-(2-Chlorophenyl)piperazine hydrochloride synthesis
- Product Name:1-(2-Chlorophenyl)piperazine hydrochloride
- CAS Number:41202-32-8
- Molecular formula:C10H14Cl2N2
- Molecular Weight:233.14
1104513-49-6
41202-32-8
To a stirred solution of tert-butyl 4-(2-chlorophenyl)piperazine-1-carboxylate (250 mg, 0.844 mmol) in 1,4-dioxane (2 mL) was added slowly and dropwise a 1,4-dioxane solution (0.9 mL, 3.60 mmol) in 4 N HCl at 0 °C. The reaction mixture was gradually warmed to room temperature and stirred continuously for 4 h (complete consumption of feedstock was confirmed by TLC monitoring). Upon completion of the reaction, the volatile solvent was removed under reduced pressure to give the crude product. The crude product was washed with ether (2 x 20 mL) and dried under high vacuum to yield 1-(2-chlorophenyl)piperazine hydrochloride (165 mg, 84% yield) as a white solid.
Yield: 96%
Reaction Conditions:
with sodium carbonate in ethanol at 80; for 25 h;
Steps:
1
Add 28.5 g (0.16 mo1) of bis (2-chloroethyl) amine hydrochloride and 200 ml of ethanol to a 500 ml three-necked flask, heat to 80 ° C, stir for 1 h, and add 21.7 g (0.17 mo1) of 2-chloroaniline , 7.4g of anhydrous sodium carbonate (0.07mo1), continue to heat and stir for 25h, cool to room temperature, suction filter, concentrate the filtrate to dryness, add 100ml of acetonitrile to crystallize, and obtain 35.8g of white crystals, yield 96%.
References:
Jiangsu Haosen Pharmaceutical Group Co., Ltd.;Cao Jin;You Junhui;Du Zuyin;Zhao Junjun;Qi Gaofei CN104829558, 2020, B Location in patent:Paragraph 0060-0062
1104513-49-6
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