HRID469364

反应详情

EQUATION

反应方程式

HRID 469364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere 0.945 g (7.35 mmol) trimethylsulphoxonium chloride were placed in 20 mL THF, and 0.300 g (7.50 mmol) sodium hydride (55%, suspension in mineral oil) were added batchwise. The reaction mixture was refluxed for 2 h. Then 1.00 g (7.35 mmol) 2-hydroxy-3-methylbenzaldehyde in 20 mL THF were added dropwise to the reaction mixture and it was refluxed overnight. Then PE was added and the suspension obtained was filtered. The filtrate was evaporated down i. vac. and purified by flash chromatography. The fractions containing the product were combined and evaporated down.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 2 h
  2. temperaturewas refluxed overnight
  3. additionThen PE was added
  4. customthe suspension obtained
  5. filtrationwas filtered
  6. customThe filtrate was evaporated down i
  7. customand purified by flash chromatography
  8. additionThe fractions containing the product
  9. customevaporated down