HRID1110706

反应详情

EQUATION

反应方程式

HRID 1110706 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of (±)-trans-2-chloro-6-propyl-5,5a,6,7,8,9,9a,10-octahydropyrido[2,3-g]quinoline hydrochloride (1.00 g, 3.32 mmol) and dimethylamine hydrochloride (15 g) was heated to 200° C. to form a homogeneous molten semi-solid. After 30 minutes, the molten semi-solid was poured into water, made basic with dilute NaOH solution, and extracted with methylene chloride. The extract was dried (Na2SO4) and concentrated to give the crude product as a brown solid. Purification by flash chromatography (10% methanol in methylene chloride, NH4OH) provided (±)-trans-2-dimethylamino-6-propyl-5,5a,6,7,8, 9,9a,10-octahydropyrido[2,3-g]quinoline (Rf =0.54, 568 mg, 63% yield) as an orange oil.

WORKUP

后处理

  1. customto form a homogeneous molten semi-solid
  2. extractionextracted with methylene chloride
  3. dry with materialThe extract was dried (Na2SO4)
  4. concentrationconcentrated
  5. customto give the crude product as a brown solid
  6. customPurification by flash chromatography (10% methanol in methylene chloride, NH4OH)