HRID1821090

反应详情

EQUATION

反应方程式

HRID 1821090 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of N1-(6-Chloro-1,2,3,4-tetrahydro-acridin-9-yl)-propane-1,3-diamine (50 mg, 0.17 mmoL), 1,5,7,8-Tetrahydro-quinoline-2,6-dione (31 mg, 0.19 mmoL) in 5 mL methylene chloride, was added sodium triacetoxyborohydride (110 mg, 0.52 mmoL) and a catalytic amount of acetic acid. After stiring at room temperature for 24 h, the reaction was stopped by adding saturated sodium bicarbonate. The mixture was extracted with methylene chloride three times. The combined methylene chloride extract was dried, filtered and concentrated. Purification by column chromatography on silica gel column with 10% MeOH/1% ammonium hydroxide in methylene chloride provided the desired product (27.6 mg, 0.063 mmoL, 37%).

WORKUP

后处理

  1. extractionThe mixture was extracted with methylene chloride three times
  2. extractionThe combined methylene chloride extract
  3. customwas dried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by column chromatography on silica gel column with 10% MeOH/1% ammonium hydroxide in methylene chloride