HRID1270288

反应详情

EQUATION

反应方程式

HRID 1270288 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a pre-cooled (0° C.) solution of the compound from Example 62, Step D (618 mg, 1.0 mmol) in THF (8 mL) was added methyl iodide (709 mg, 5.0 mmol) and NaH (60% in mineral oil) (44 mg, 1.1 mmol). The resulting mixture was stirred overnight at rt and then poured into a stirred mixture of saturated aqueous ammonium chloride (50 mL) and dichloromethane (50 mL). The organic layer was washed with water (50 mL), dried (MgSO4) and evaporated in vacuo. The resulting crude product was purified on silica gel using ethyl acetate/hexane as the eluent. Fractions containing the product were pooled and evaporated in vacuo to give the desired product (735 mg) as a colorless foam.

WORKUP

后处理

  1. washThe organic layer was washed with water (50 mL)
  2. dry with materialdried (MgSO4)
  3. customevaporated in vacuo
  4. customThe resulting crude product was purified on silica gel
  5. additionFractions containing the product
  6. customevaporated in vacuo