HRID2192220

反应详情

EQUATION

反应方程式

HRID 2192220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2e (40 mg, 0.168 mmol) in CH2Cl2 was added benzoyl isothiocyanate (30 mg, 0.189 mmol). The reaction mixture was kept at reflux for 2.5 h. The reaction mixture was filtered through a cake of Celite® and washed the cake with CH2Cl2. The solvent was evaporated under reduced pressure. The desired product was purified by column chromatography using 0 to 80% EtOAc in hexane over 60 min as eluting gradient to afford 2f (76 mg, 99%) as a powder. MS (ES) m/z 402 [M+H]+.

WORKUP

后处理

  1. temperatureat reflux for 2.5 h
  2. filtrationThe reaction mixture was filtered through a cake of Celite®
  3. washwashed the cake with CH2Cl2
  4. customThe solvent was evaporated under reduced pressure
  5. customThe desired product was purified by column chromatography
  6. customover 60 min
  7. washas eluting gradient