HRID1012653

反应详情

EQUATION

反应方程式

HRID 1012653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Compound 508 (1.5 g, 10.7 mmol) was dissolved in dry DMF (40 mL) under an argon atmosphere. tert-Butyl-chloro-dimethyl-silane (2.43 g, 16.1 mmol) and imidazole (1.1 g, 16.1 mmol) was added. Stirred at RT for 2 h, added EtOAc (250 mL) and then washed with water (2×100 mL), 4% MgSO4 (2×75 mL), dried (MgSO4), filtered, and concentrated in vacuo to afford the crude product as yellow oil. Purified by chromatography using EtOAc/petroleum ether (40-60)(1:20) as the eluent, affording the title compound as an colourless, clear oil.

WORKUP

后处理

  1. washwashed with water (2×100 mL), 4% MgSO4 (2×75 mL)
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto afford the crude product as yellow oil
  6. customPurified by chromatography