反应详情

To a solution of 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide (150 mg) in anhydrous pyridine (3 mL) was added trans-4-aminocyclohexanol (81.4 mg), and the mixture was stirred for 15 hours at ambient temperature, and then for 3 hours at 60° C. The mixture was partitioned between ethyl acetate and water. The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was subjected to a silica gel column chromatography eluting with a mixture of chloroform and methanol (20:1). The eluent was concentrated and the residue was triturated with diisopropyl ether to give 2-(trans-4-hydroxycyclohexylamino)-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide as yellow powders (164 mg).

1. waitfor 3 hours at 60° C
2. customThe mixture was partitioned between ethyl acetate and water
3. washThe separated organic layer was washed with water and brine
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. washeluting with a mixture of chloroform and methanol (20:1)
7. concentrationThe eluent was concentrated
8. customthe residue was triturated with diisopropyl ether