反应详情

13 mg (E)-N-(3-(1-methyl-1H-tetrazol-5-ylthio)-4-oxonaphthalen-1(4H)-ylidene)thiophene-2-sulfonamide (13d) was dissolved in 50 ml ethyl acetate, to which was added 27 mg sodium hydrosulfite solid followed by 10 ml water. The mixture was shaken in a separation funnel until the yellow organic phase turned colorless. The organic phase was separated and washed with water and brine. Dried over Na2SO4, the organic phase was filtered and the filtrate was concentrated to dryness. The residue was dissolved in dichloromethylene and triturated with hexane. The precipitate was washed with dichloromethylene/hexane (1:1) affording the title compound 13 mg (99%) as a white solid, m.p.: 130° C. (dec.).

1. customThe organic phase was separated
2. washwashed with water and brine
3. dry with materialDried over Na2SO4
4. filtrationthe organic phase was filtered
5. concentrationthe filtrate was concentrated to dryness
6. dissolutionThe residue was dissolved in dichloromethylene
7. customtriturated with hexane
8. washThe precipitate was washed with dichloromethylene/hexane (1:1)