反应详情

To 200 mL of a suspension of 5.21 g of LAH in THF cooled with ice was added dropwise, under argon flow, 50 mL of a solution of 25.5 g of 2-methoxy-4-[(4-methylpiperazin-1-yl)methyl]benzoic acid methyl ester in THF. The mixture was stirred under ice cooling for 1 hour and further stirred at room temperature for 22 hours. To the reaction mixture cooled with ice, 25 mL of a 10% NaOH water was added dropwise. After 30-minute stirring, the mixture was filtered through Celite. The filtrate was washed with 150 mL of THF and then was concentrated. To the residue, 50 mL of saturated brine and 300 mL of dichloromethane were added, and the organic layer was separated. The organic layer was concentrated. The residue was purified by silica gel column chromatography (CHCl3/methanol system) to give 22.4 g of the title compound (98% yield).

1. stirringfurther stirred at room temperature for 22 hours
2. additionwas added dropwise
3. stirringAfter 30-minute stirring
4. filtrationthe mixture was filtered through Celite
5. washThe filtrate was washed with 150 mL of THF
6. concentrationwas concentrated
7. additionTo the residue, 50 mL of saturated brine and 300 mL of dichloromethane were added
8. customthe organic layer was separated
9. concentrationThe organic layer was concentrated
10. customThe residue was purified by silica gel column chromatography (CHCl3/methanol system)