HRID327464
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
PROCEDURE
实验过程
Di (2-pyridyl)thiocarbonate (1.6 g, 7.2 mmol) was added to a stirred solution of 1,2,3,4-tetrahydro-N3,N3 -dipropyl-3,8-quinolinediamine (1.6 g, 6.7 mmol) in THF (50 mL). The solution was stirred for 1 hour, evaporated, and partitioned between chloroform and water. The chloroform phase was evaporated and chromatographed on silica gel using ethyl acetate:hexane (1:9) as the initial eluant to give 1.6 g of product. Crystallization from cyclohexane gave 1.3 g (67% of 5-(dipropylamino)-5,6-hydro-4H-imidazo(4,5,1-ij)quinolin-2(1H)-thione, mp 150°-151° C. Anal. Calcd. for C16H23N3S: C, 66.39; H, 8.01; N, 14.52; S, 11.08. Found: C, 66.50; H, 8.18; N, 14.56; S, 11.02.
WORKUP
后处理
- customevaporated
- custompartitioned between chloroform and water
- customThe chloroform phase was evaporated
- customchromatographed on silica gel