反应 #42679

反应方程式

sodium sulfate decahydrate

lithium aluminum hydride

3,5-dichloro-4-aminobenzonitrile

→

3,5-dichloro-4-aminobenzylamine

溶剂

THF

THF

反应条件

后处理

1. 1
   workup.STIRRINGstirred for 30 min
2. 2
   过滤The solid was filtered off
3. 3
   洗涤washed with THF for three times
4. 4
   其他The solvent was removed by rotovap and residue
5. 5
   其他was purified by column with Methanol/DCM (3:7) as the eluant

实验过程

To lithium aluminum hydride (0.57 g, 15 mmol) in dry THF (20 mL) was added dropwise 3,5-dichloro-4-aminobenzonitrile (1.87 g, 10 mmol) in THF (30 mL). The mixture was stirred at RT for 2 hours. Then, sodium sulfate decahydrate (4.83 g, 15 mmol) was added and stirred for 30 min. The solid was filtered off and washed with THF for three times. The solvent was removed by rotovap and residue was purified by column with Methanol/DCM (3:7) as the eluant. 3,5-dichloro-4-aminobenzylamine was obtained as an off-white solid (1.5 g, 80%). 1H NMR (300 MHz, CD3OD): δ 7.2 (s, 2H), 3.65 (s, 2H).

来源