반응 #170164

ord-8470f77bc3454ea2b731c5f16d4126ae

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타1 hour
  2. 2
    기타at 70° C
  3. 3
    온도After cooling down to room temperature
  4. 4
    workup.STIRRINGthe reaction mixture was stirred at 70° C. for 1 hour
  5. 5
    농축After concentration to dryness
  6. 6
    기타the crude mixture was triturated in pentane (2×15 mL)
  7. 7
    기타to give a yellow oil (698 mg, quantitative) which
  8. 8
    기타was used in the next step without further purification

실험 절차

1-Chloroethylchloroformate (361 μL, 3.33 mmol) was added to a solution of 1-benzhydryl-3-(2-(thiophen-2-yl)ethoxy)azetidine (1.11 g, 3.17 mmol) in dichloromethane (15 mL) at room temperature. The reaction mixture was stirred overnight at room temperature, then 1 hour at 70° C. After cooling down to room temperature, ethanol (15 mL) was added and the reaction mixture was stirred at 70° C. for 1 hour. After concentration to dryness, the crude mixture was triturated in pentane (2×15 mL) to give a yellow oil (698 mg, quantitative) which was used in the next step without further purification.

출처

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