HRID1516755

反应详情

EQUATION

反应方程式

HRID 1516755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of lithium aluminium hydride (36 ml; 1N in THF) is added dropwise to a solution of N,N-bis(3-methylbutyl)-4-nitro-3-[(3-piperidin-1-ylpropyl)amino]benzamide (1.6 g) cooled down to 0° C. The mixture is taken to a temperature of 20° C. then heated under reflux for 6 hours and hydrolyzed with water cooled down to 0° C. followed by a 1N soda solution. After the addition of dichloromethane, the mixture is filtered on celite. After decantation of the filtrate and extractions, the combined organic phases are washed with 1N soda then with salt water, dried over Na2SO4 and concentrated under reduced pressure at 40° C. in order to produce the expected compound in the form of an oil (1.23 g, 85% yield).

WORKUP

后处理

  1. customis taken to a temperature of 20° C.
  2. temperaturethen heated
  3. temperaturecooled down to 0° C.
  4. filtrationthe mixture is filtered on celite
  5. extractionAfter decantation of the filtrate and extractions
  6. washthe combined organic phases are washed with 1N soda
  7. dry with materialwith salt water, dried over Na2SO4
  8. concentrationconcentrated under reduced pressure at 40° C. in order