反应详情

To a solution of methyl 5-methanesulfonyl-2-(morpholin-4-yl)benzoate obtained in Step 3 in tetrahydrofuran (300 ml) was added lithium aluminum hydride (3.6 g, 94 mmol) by small portions under ice-cooling. After stirring under ice-cooling for 1 hr, 1N hydrochloric acid (200 ml) was slowly added and the mixture was stirred at room temperature for 1 hr. After extraction with ethyl acetate (500 ml), the organic layer was washed with saturated brine (200 ml×3), and dried over magnesium sulfate. After filtration and concentration, the resulting solid was collected by filtration. The solid was washed with a mixed solvent (100 ml) of hexane-ethyl acetate (4:1) to give 5-methanesulfonyl-2-(morpholin-4-yl)benzyl alcohol (8.6 g, yield 34%).

1. temperaturecooling
2. temperaturecooling for 1 hr
3. stirringthe mixture was stirred at room temperature for 1 hr
4. extractionAfter extraction with ethyl acetate (500 ml)
5. washthe organic layer was washed with saturated brine (200 ml×3)
6. dry with materialdried over magnesium sulfate
7. filtrationAfter filtration and concentration
8. filtrationthe resulting solid was collected by filtration
9. washThe solid was washed with a mixed solvent (100 ml) of hexane-ethyl acetate (4:1)