反应详情

Step N4. To above methyl 3-carbamoyl-5-chlorobenzoate (˜9.3 mmol) in dry THF (100 mL) was added lithium aluminum hydride (1 g, 26.3 mmol) in portions. The mixture was stirred for 4 hours, then treated with sodium sulfate decahydrate (8.5 g, 26.3 mmol) for 30 min. The solid was filtered off and washed with THF for three times. The solvent was removed under vacuum and resulting residue was purified by column with DCM, then MeOH/DCM (5/95) to give 3-chloro-5-(hydroxymethyl)benzamide (13, 0.7 g, 40%).

1. filtrationThe solid was filtered off
2. washwashed with THF for three times
3. customThe solvent was removed under vacuum
4. customresulting residue
5. customwas purified by column with DCM