HRID1492629

反应详情

EQUATION

反应方程式

HRID 1492629 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 2.34 g (7.45 mmol) of the product of Step J in DMF (30 mL) were added imidazole (609 mg, 8.94 mmol) and tertbutyldimethyl-chlorosilane (1.35 g, 8.94 mmol) at 0° C. The solution was stirred at room temperature for 18 hours, and was then poured into 100 mL of ethyl acetate and washed with H2O (2×). The water layer was extracted with ethyl acetate (2×). The combined organic layer was washed with H2O (3×) and brine, and was dried over anhydrous MgSO4. After concentration the mixture was purified by flash chromatography (hexane: EtOAc=10:1) to give 1.96 g of the title compound as a clear oil.

WORKUP

后处理

  1. washwashed with H2O (2×)
  2. extractionThe water layer was extracted with ethyl acetate (2×)
  3. washThe combined organic layer was washed with H2O (3×) and brine
  4. dry with materialwas dried over anhydrous MgSO4
  5. concentrationAfter concentration the mixture
  6. customwas purified by flash chromatography (hexane: EtOAc=10:1)