反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- addition1 N Borane tetrahydrofuran complex (13 ml) was added dropwise
- temperatureThe reaction mixture was cooled again to 0° C.
- temperatureby heating to 50° C
- extractionThe reaction solution was extracted with ethyl acetate
- extractionextracted with chloroform
- washThe extract was washed with a saturated saline solution
- dry with materialdried over sodium sulfate anhydrous
- concentrationThe product was concentrated under reduced pressure