HRID1393648

反应详情

EQUATION

反应方程式

HRID 1393648 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

The N-benzyl-4-methyl-4-nitropentanoic acid amide (2.5 g) obtained above was dissolved in tetrahydrofuran (20 ml) and cooled to 0° C. 1 N Borane tetrahydrofuran complex (13 ml) was added dropwise thereto and then stirred overnight at room temperature. The reaction mixture was cooled again to 0° C., and 2 N hydrochloric acid (30 ml) was added thereto, followed by heating to 50° C. The reaction solution was extracted with ethyl acetate. The aqueous phase was alkalinized by 50% sodium hydroxide solution, extracted with chloroform. The extract was washed with a saturated saline solution, and dried over sodium sulfate anhydrous. The product was concentrated under reduced pressure to give benzyl-4-methyl-4-nitropentylamine (1.7 g, Y.: 73%) as a colorless oil.

WORKUP

后处理

  1. addition1 N Borane tetrahydrofuran complex (13 ml) was added dropwise
  2. temperatureThe reaction mixture was cooled again to 0° C.
  3. temperatureby heating to 50° C
  4. extractionThe reaction solution was extracted with ethyl acetate
  5. extractionextracted with chloroform
  6. washThe extract was washed with a saturated saline solution
  7. dry with materialdried over sodium sulfate anhydrous
  8. concentrationThe product was concentrated under reduced pressure