HRID970299

反应详情

EQUATION

反应方程式

HRID 970299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium thiocyanate (2.81 g, 28.7 mmol), tetrabutylammonium hydrogen sulphate (1.22 g, 3.59 mmol) and molecular sieves (6.00 g) were stirred in absolute acetonitrile (500 ml) for 30 minutes. 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl bromide 37 (5.90 g, 14.4 mmol) was then dissolved in acetonitrile, added to the reaction flask and refluxed for 90 minutes. The solution was then allowed to cool, filtered through a celite pad and concentrated. Purification by column chromatography in hexane:ethyl acetate 2:1 (v/v) to give 52 (4.26 g, 76%).

WORKUP

后处理

  1. additionadded to the reaction flask
  2. temperaturerefluxed for 90 minutes
  3. temperatureto cool
  4. filtrationfiltered through a celite pad
  5. concentrationconcentrated
  6. customPurification by column chromatography in hexane:ethyl acetate 2:1 (v/v)