HRID1084694
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customto form a homogeneous molten semi-solid
- extractionextracted with methylene chloride
- dry with materialThe extract was dried (Na2SO4)
- concentrationconcentrated
- customto give the crude product as a brown solid
- customPurification by flash chromatography (10% methanol in methylene chloride, NH4OH)