تفاعل #1688

معادلة التفاعل

NaBH4

p-BocNHCH2C6H4NO2

NaBH4

→

white solid

المردود 97.0%

p-BocNHCH2C6H4NH2

المردود 97.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىthe solvent was evaporated in vacuo
2. 2
   workup.DISSOLUTIONthe residue was dissolved in conc. ammonium hydroxide
3. 3
   استخلاصextracted twice with dichloromethane
4. 4
   غسيلThe combined organic extracts were washed with brine
5. 5
   تجفيفdried with MgSO4
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated in vacuo

الإجراء التجريبي

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.

المصدر