HRID2067148

反应详情

EQUATION

反应方程式

HRID 2067148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of cannabidiol (125.8 mg, 0.4 mmol) and (t-butyldimethylsilyloxy)acetic acid (112.9 mg, 0.51 mmol) in dry dichloromethane (1 mL) was added of 4-dimethylaminopyridine (6.2 mg, 0.03 mmol) followed by N,N′-dicyclohexylcarbodiimide (123.8 mg, 0.6 mmol). The mixture was stirred at ambient temperature for 1 h. Additional amounts of the acid (26.6 mg) and N,N′-dicyclohexylcarbodiimide (31 mg) were added and stirring was continued for 1 h. Mixture was diluted with hexane (2 mL), filtered, and concentrated. The crude product was purified by preparative reverse phase HPLC (C8 column) with acetonitrile-water to afford cannabidiol (t-butyldimethylsilyloxy)acetate as an oil.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 1 h
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude product was purified by preparative reverse phase HPLC (C8 column) with acetonitrile-water