HRID1648300
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
Sodium cyanoborohydride (0.17 g) was added in small portions over a 5-hour period to a stirred solution of 1.90 g (8.4 retool) 5-amino-5,6-dihydro-4H-imidazo(4,5,1-ij) quinolin-2(1H)-one, 0.85 mL sodium methoxide and 1.5 g propionaldehyde in methanol (175 mL). Methanolic ammonia solution was added, and after 30 minutes, the solvent was evaporated. The residual oil was partitioned between ethyl acetate and water and the crude product obtained by evaporating the ethyl acetate was dissolved in chloroform and chromatographed on silica gel eluting with 2.5% methanol:chloroform to give 1.24 g (64% yield) of 5,6-dihydro-5-(propylamino)-4H-imidazo(4,5,1-ij)quinolin-2(1H)-one.
WORKUP
后处理
- customthe solvent was evaporated
- customThe residual oil was partitioned between ethyl acetate and water
- customthe crude product obtained
- customby evaporating the ethyl acetate
- dissolutionwas dissolved in chloroform
- customchromatographed on silica gel eluting with 2.5% methanol