反应 #1688

反应方程式

NaBH4

p-BocNHCH2C6H4NO2

NaBH4

→

white solid

收率 97.0%

p-BocNHCH2C6H4NH2

收率 97.0%

溶剂

methanol

反应条件

后处理

1. 1
   其他the solvent was evaporated in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in conc. ammonium hydroxide
3. 3
   萃取extracted twice with dichloromethane
4. 4
   洗涤The combined organic extracts were washed with brine
5. 5
   干燥dried with MgSO4
6. 6
   过滤filtered
7. 7
   浓缩concentrated in vacuo

实验过程

To a stirring solution of p-BocNHCH2C6H4NO2 (7.5 g, 29.7 mmol) and NiCl2.6H2O (17.7 g, 74.3 mmol) in methanol (150 mL) at 0° C. was added NaBH4 (5.6 g, 149 mmol) in small portions over 30 min. After complete addition of NaBH4 and 15 min, the solvent was evaporated in vacuo and the residue was dissolved in conc. ammonium hydroxide and extracted twice with dichloromethane. The combined organic extracts were washed with brine, dried with MgSO4, filtered and concentrated in vacuo to give 6.4 g (97%) of a white solid.

来源