HRID471303

反应详情

EQUATION

反应方程式

HRID 471303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-chlorosuccinimide (0.83 g) was added portionwise to a solution of tert-butyldimethyl(2-(thiophen-2-yl)ethoxy)silane (1.5 g) (example 4 step a) in chloroform (50 mL) and heated to reflux for 3 days. The yellow solution was diluted with DCM (100 mL) and washed with saturated sodium bicarbonate solution (2×100 mL), brine (100 mL), dried over sodium sulphate, filtered and evaporated in vacuo. The residue was purified by silica gel chromatography eluting with iso-hexane. The fractions containing product were combined and evaporated in vacuo to give the subtitled compound as a clear oil. Yield 1 g.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 3 days
  3. washwashed with saturated sodium bicarbonate solution (2×100 mL), brine (100 mL)
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customThe residue was purified by silica gel chromatography
  8. washeluting with iso-hexane
  9. additionThe fractions containing product
  10. customevaporated in vacuo