Reacción #42679

Ecuación de reacción

sodium sulfate decahydrate

lithium aluminum hydride

3,5-dichloro-4-aminobenzonitrile

→

3,5-dichloro-4-aminobenzylamine

Disolventes

THF

THF

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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).

Fuente