HRID33231

反应详情

EQUATION

反应方程式

HRID 33231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(4-Methyl-5-quinolin-6-yl-4H-[1,2,4]triazol-3-ylsulfanyl)-butyraldehyde (0.1 g, 0.32 mmol) and 7-Ethanesulfonyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.11 g, 0.45 mmol) were stirred at room temperature in dichloromethane (4 ml) for 20 min. Sodium triacetoxyborohydride (71 mg, 0.34 mmol) was then added and the mixture stirred overnight. The mixture was diluted with dichloromethane (50 ml) and washed with saturated sodium bicarbonate solution (30 ml). The aqueous was extracted with further dichloromethane (50 ml) and the combined organic portions were dried (Na2SO4), filtered and evaporated to give a yellow oil. Purification by silica gel chromatography (eluent 10% MeOH:EtOAc) which gave the title compound as a colourless oil (35 mg, 21%).

WORKUP

后处理

  1. washwashed with saturated sodium bicarbonate solution (30 ml)
  2. extractionThe aqueous was extracted with further dichloromethane (50 ml)
  3. dry with materialthe combined organic portions were dried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated
  6. customto give a yellow oil
  7. customPurification by silica gel chromatography (eluent 10% MeOH:EtOAc) which