HRID1918317

反应详情

EQUATION

反应方程式

HRID 1918317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound of step 1 (20 g, 89.2 mmol) was dissolved in DMF (100 ml) and cooled in an ice bath. Potassium carbonate (18.4 g, 134 mmol) and, immediately thereafter, benzyl bromide (15.2 g, 89.2 mmol) were added. This mixture was stirred for 30 min at room temperature, poured on a mixture of 2 N hydrochloric acid and diethyl ether, filtered and washed repeatedly with diethyl ether. The combined ethereal phases were washed with water, dried over sodium chloride, decanted and evaporated to dryness. The residue was purified by silica gel chromatography (HEP/EA gradient) to yield the title compound (21 g).

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. filtrationfiltered
  3. washwashed repeatedly with diethyl ether
  4. washThe combined ethereal phases were washed with water
  5. dry with materialdried over sodium chloride
  6. customdecanted
  7. customevaporated to dryness
  8. customThe residue was purified by silica gel chromatography (HEP/EA gradient)