HRID1648300

反应详情

EQUATION

反应方程式

HRID 1648300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customthe solvent was evaporated
  2. customThe residual oil was partitioned between ethyl acetate and water
  3. customthe crude product obtained
  4. customby evaporating the ethyl acetate
  5. dissolutionwas dissolved in chloroform
  6. customchromatographed on silica gel eluting with 2.5% methanol