HRID1461279

反应详情

EQUATION

反应方程式

HRID 1461279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5,6-dihydroquinoline (9.17g, 0.07 mmol) in methanol (10 ml) at 0° was treated portionwise with N-methylhydroxylamine hydrochloride (11.5 g, 0.138 mmol), stirred for 2h, poured into saturated aqueous sodium bicarbonate (250 ml), and extracted with chloroform (3 x 150 ml). The extracts were washed with water (50 ml), dried (MgSO4), and evaporated in vacuo. The residual brown liquid was purified by chromatography (alumina; ether) to give the product (6.45 g) as a colorless oil, which was converted into the amine of Example 2.

WORKUP

后处理

  1. extractionextracted with chloroform (3 x 150 ml)
  2. washThe extracts were washed with water (50 ml)
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo
  5. customThe residual brown liquid was purified by chromatography (alumina; ether)