HRID448694

反应详情

EQUATION

反应方程式

HRID 448694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To an ice-cold mixture of the product from Step A (475 mg, 0.7 mmol) in THF (7 mL) was added NaH (60% in mineral oil, 29 mg) and stirred at 0° C. for 0.5 h. Then MeI (48 μL) was added and reaction mixture stirred at rt for 24 h. The reaction was quenched with MeOH and the mixture evaporated. The crude product was purified on a silica gel column (5×3.5 cm) using hexane/ethyl acetate (9/1, 7/1, 5/1 and 3/1) as eluent. Fractions containing the product were combined and evaporated to give the desired compound (200 mg) as a colorless foam.

WORKUP

后处理

  1. customreaction mixture
  2. stirringstirred at rt for 24 h
  3. customThe reaction was quenched with MeOH
  4. customthe mixture evaporated
  5. customThe crude product was purified on a silica gel column (5×3.5 cm)
  6. additionFractions containing the product
  7. customevaporated