반응 #1703170
ord-44e6058fb35b40f39c6b435c0fc2c8c9
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시약
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후처리
- 1workup.WAITthen left
- 2workup.WAITto stand for 3 days
- 3workup.STIRRINGstirred at 20° C. for 20 h
- 4여과The solution was filtered through a filter tube
- 5세척the residue washed with methanol (5 ml)
- 6기타the combined filtrates were evaporated to dryness
- 7기타to give a yellow solid
- 8workup.DISSOLUTIONthe solid dissolved
- 9기타The organic phase was separated
- 10건조dried with sodium sulphate
- 11여과filtered
- 12기타then evaporated
- 13기타to give a pale yellow solid
- 14workup.DISSOLUTIONsome white solid did not dissolve
- 15기타to give a yellow solid which
- 16기타DMSO (1 ml) and purified by mass
- 17기타The residue was azeotroped with methanol (5 ml)
실험 절차
A mixture of 6-bromo-3-fluoro-4-nitro-1H-indazole and 6-bromo-4-nitro-1H-indazole (3:2) (187 mg) was dissolved in methanol (6 ml) and water (1.2 ml) and treated with sodium dithionate (519 mg). The solution was stirred for 2 h at 20° C. then left to stand for 3 days. This solution was then treated with sodium dithionite (438 mg) and stirred at 20° C. for 20 h. The solution was filtered through a filter tube, the residue washed with methanol (5 ml) then the combined filtrates were evaporated to dryness to give a yellow solid. This was treated with ethyl acetate (10 ml) and water (10 ml) and the solid dissolved. The organic phase was separated, dried with sodium sulphate, filtered then evaporated to give a pale yellow solid. This solid was treated with DCM (5 ml), methanol (5 ml) and ethyl acetate (10 ml), but some white solid did not dissolve. The supernatant was pipetted off, then blown to dryness to give a yellow solid which was dissolved in 1:1 methanol:DMSO (1 ml) and purified by mass directed preparative HPLC (Method A). The residue was azeotroped with methanol (5 ml) to give the title compound (19 mg) as a white solid.