반응 #1688

반응 방정식

NaBH4

p-BocNHCH2C6H4NO2

NaBH4

→

white solid

수율 97.0%

p-BocNHCH2C6H4NH2

수율 97.0%

용매

methanol

반응 조건

후처리

1. 1
   기타the solvent was evaporated in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in conc. ammonium hydroxide
3. 3
   추출extracted twice with dichloromethane
4. 4
   세척The combined organic extracts were washed with brine
5. 5
   건조dried with MgSO4
6. 6
   여과filtered
7. 7
   농축concentrated in vacuo

실험 절차

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.

출처