反应详情

N-[5-(3,5-Difluoro-benzoyl)-1H-indazol-3-yl]-4-(4-methyl-piperazin-1-yl)-2-nitro-benzamide (3.61 g, 6.93 mmol) was dissolved in DCM (150 mL) in argon atmosphere and trifluoroacetic acid (150 mL) is added under stirring. Sodium borohydride pellets (2.62 gr, 69.3 mmol) is gradually added over a period of 72 hours. The reaction mixture was evaporated, taken up with a mixture MeOH/acetone and stirred for 1 hour. The resulting mixture was evaporated to dryness, redissolved in MeOH and NaOH 8N was added till basic pH was reached. Crude was evaporated and ice/water was added, the solid thus formed was filtered, washed with water and dried under vacuum at 80° C. affording 3.22 g of title compound (92% yield).

1. additionis added
2. additionis gradually added over a period of 72 hours
3. customThe reaction mixture was evaporated
4. stirringstirred for 1 hour
5. customThe resulting mixture was evaporated to dryness
6. dissolutionredissolved in MeOH
7. additionNaOH 8N was added till basic pH
8. customCrude was evaporated
9. additionice/water was added
10. customthe solid thus formed
11. filtrationwas filtered
12. washwashed with water
13. customdried under vacuum at 80° C.