反応 #1688

反応方程式

NaBH4

p-BocNHCH2C6H4NO2

NaBH4

→

white solid

収率 97.0%

p-BocNHCH2C6H4NH2

収率 97.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他the solvent was evaporated in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in conc. ammonium hydroxide
3. 3
   抽出extracted twice with dichloromethane
4. 4
   洗浄The combined organic extracts were washed with brine
5. 5
   乾燥dried with MgSO4
6. 6
   ろ過filtered
7. 7
   濃縮concentrated in vacuo

実験手順

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.

出典