반응 #721068

ord-590b7d12837c40bea8e83e4d76df40e8

용매

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling to room temperature
  2. 2
    workup.STIRRINGthe reaction mixture was stirred at 70° C. for 1.5 h
  3. 3
    농축The reaction mixture was concentrated to dryness
  4. 4
    기타The crude mixture was triturated in pentane
  5. 5
    기타to give a dark wax (140 mg, quantitative) which
  6. 6
    기타was used without further purification

실험 절차

A 50 mL flask was charged with 1-(diphenylmethyl)-3-(2-thienylmethoxy)azetidine (204 mg, 0.61 mmol; which may be prepared as described in Step 2) and 1,2-dichloroethane (2.7 mL). 1-Chloroethyl chloroformate (86 μL, 0.79 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (2.7 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was concentrated to dryness. The crude mixture was triturated in pentane to give a dark wax (140 mg, quantitative) which was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09321769B2uspto-grants-2016_04