반응 #170229

반응 방정식

1-Chloroethyl chloroformate

1-benzhydryl-3-((4-bromothiophen-2-yl)methoxy)-azetidine

Ethanol

→

solid

수율 77.0%

3-((4-Bromothiophen-2-yl)methoxy)-azetidine hydrochloride

수율 77.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction mixture was stirred overnight
2. 2
   농축After concentration to dryness
3. 3
   기타the crude mixture was precipitated from a mixture dichloromethane/diethyl ether

실험 절차

1-Chloroethyl chloroformate (218 μL, 2.0 mmol) was added to a solution of 1-benzhydryl-3-((4-bromothiophen-2-yl)methoxy)-azetidine (793 mg, 1.91 mmol) in dichloromethane (10 mL). The reaction mixture was stirred for 1 hour at 0° C. and for an additional 1 hour at room temperature. Ethanol (10 mL) was then added and the reaction mixture was stirred overnight. After concentration to dryness, the crude mixture was precipitated from a mixture dichloromethane/diethyl ether to afford a white solid (417 mg, 77%) which was used in the next step whitout further purification.

출처