HRID434763

反应详情

EQUATION

反应方程式

HRID 434763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 10 ml of dichloromethane is added 0.5 g. (3.73 mmoles) of cinnamyl alcohol. The resulting mixture is added to a stirred suspension of 3.37 g. (11.5 mmoles) of 2,2'-bipyridinium chlorochromate in 15 ml of dichloromethane. The resulting mixture is stirred for four hours after which 15 ml of anhydrous ether is added. The resulting product is filtered through a Hirsch funnel packed 1-2 cm deep with Celite® using ether as a wash solvent. The resulting clear filtrate is washed with 5% hydrochloric acid and 10% sodium carbonate, and dried over sodium sulfate. The drying agent is removed and the solvent evaporated giving a product which is a slightly yellow oil. This oil is then distilled via Kugelrohr to yield pure cinnamaldehyde in a typical yield of 0.323 g. which is 86% of theoretical yield.

WORKUP

后处理

  1. additionThe resulting mixture is added to a stirred suspension of 3.37 g
  2. additionis added
  3. filtrationThe resulting product is filtered through a Hirsch funnel
  4. washThe resulting clear filtrate is washed with 5% hydrochloric acid and 10% sodium carbonate
  5. dry with materialdried over sodium sulfate
  6. customThe drying agent is removed
  7. customthe solvent evaporated
  8. customgiving a product which
  9. distillationThis oil is then distilled via Kugelrohr