HRID365497

反应详情

EQUATION

反应方程式

HRID 365497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

36.40 g (139 mmol) of triphenylphosphine are added, all at once and with vigorous stirring, to a solution, cooled to 0° C., of 10.40 g (70 mmol) of 2-hydroxymethyl-benzo[b]furan and 46 g (139 mol) of CBr4 in 220 ml of ether. After stirring for 4 hours at 20° C., the precipitate formed is suctioned off and washed with Et2O; the filtrate is dried and concentrated, and the residue is then chromatographed on silica, eluting with a mixture of cyclohexane/CH2Cl2 =80/20, to yield the expected compound in the form of an oil.

WORKUP

后处理

  1. customthe precipitate formed
  2. washwashed with Et2O
  3. customthe filtrate is dried
  4. concentrationconcentrated
  5. customthe residue is then chromatographed on silica
  6. washeluting with a mixture of cyclohexane/CH2Cl2 =80/20