反応 #1072046

ord-aaea633f0c834cf595afa98006f11875

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGAfter stirring at 0° C. for additional 30 min
  2. 2
    濃縮the reaction mixture was concentrated in vacuo
  3. 3
    その他The crude material was purified by preparative HPLC

実験手順

To a solution of Example 29 (25 mg, 0.0625 mmol) in dichloromethane at 0° C. was added m-CPBA (77%, 14 mg, 0.0625 mmol). After stirring the mixture at 0° C. for 30 min, triphenylphosphine (5 mg, 0.019 mmol) was added. After stirring at 0° C. for additional 30 min, the reaction mixture was concentrated in vacuo. The crude material was purified by preparative HPLC to afford the title compound (11 mg, 42% yield) as a white solid. MS: (M+H)+=417.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06869952B2uspto-grants-2005_03