HRID1276541

反应详情

EQUATION

反应方程式

HRID 1276541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(1,2,3,5,6,7-Hexahydro-s-indacen-4-yl)-ethanone (33 grams), ethanol (250 mL) hydroxylamine hydrochloride (58.5 grams) and pyridine (80 mL) was heated to reflux for a period of 12 hours. The mixture was then cooled to room temperature and concentrated in vacuo. The residue was then treated with 500 mL of water and extracted with chloroform-methanol. The organic phase was dried over anhydrous sodium sulfate and concentrated in vacuo to afford 32 grams of the title compound as a mixture of E and Z isomers, 178.6-182.3° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for a period of 12 hours
  3. concentrationconcentrated in vacuo
  4. additionThe residue was then treated with 500 mL of water
  5. extractionextracted with chloroform-methanol
  6. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuo