반응 #170231

ord-91ac5fbd3cf542568951fb6fbaf4c626

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

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-chlorothiophen-2-yl)methoxy)-azetidine (793 mg, 1.91 mmol) in dichloromethane (10 mL) at 0° C. The reaction mixture was stirred for 1 hour at 0° C. and for an additional 1 hour at room temperature. Ethanol (10 mL) was 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 the title compound as a white solid (417 mg, 77%) which was used whitout further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846711B2uspto-grants-2014_09