1-(2-CHLOROETHYL)-4-[3-(TRIFLUOROMETHYL)PHENYL]PIPERAZINE DIHYDROCHLORIDE synthesis
- Product Name:1-(2-CHLOROETHYL)-4-[3-(TRIFLUOROMETHYL)PHENYL]PIPERAZINE DIHYDROCHLORIDE
- CAS Number:57061-71-9
- Molecular formula:C13H16ClF3N2
- Molecular Weight:292.73
40004-29-3
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Yield:57061-71-9 96%
Reaction Conditions:
with dichlorosulfoxide in dichloromethane; for 2 h;Cooling with ice;Reflux;Reagent/catalyst;Solvent;
Steps:
17.1; 17.2; 17.3 Preparation of intermediate II
(1) 500ml reaction flask added2- (4- (3-trifluoromethylphenyl) piperazine-1-ethanol (33.0 g, 0.12 mol),DCM (330ml),Stirring, ice-water bath cooling,The DCM used in this patent is methylene chloride;(2) A solution of thionyl chloride (57.0 g, 0.479 mol) in DCM (30 ml) was added dropwise,After heating plus reflux 2h;(3) the reaction was concentrated under reduced pressure,The concentrated product was recrystallized from ethanol,38.0 g of white solid powder was obtained,The yield of Intermediate II was 96%.
References:
CN106866582,2017,A Location in patent:Paragraph 0036; 0037; 0038; 0039; 0040; 0041; 0042-0044
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