反应详情

33.8 mg (E)-N-(3-(1-methyl-1H-tetrazol-5-ylthio)-4-oxonaphthalen-1(4H)-ylidene)thiophene-2-sulfonamide (12a) was dissolved in 3 ml THF, to which was added 13.7 mg 3-aminobenzoic acid. The resulting orange solution was stirred at r.t. for 30 min and 0.2 ml THF solution containing 1 eq. pyridine was added. The reaction was continued for 30 min. The mixture was diluted to 50 ml with ethyl acetate and washed with 0.5 N NaHSO4 solution, water and brine. Dried over Na2SO4, the organic phase was filtered and the filtrate was concentrated. The residue was washed with dichloromethylene/hexane (1:1) affording the title compound 32.5 mg (74.2%) as a red solid, m.p.: 230° C. (dec.).

1. additionwas added
2. waitThe reaction was continued for 30 min
3. washwashed with 0.5 N NaHSO4 solution, water and brine
4. dry with materialDried over Na2SO4
5. filtrationthe organic phase was filtered
6. concentrationthe filtrate was concentrated
7. washThe residue was washed with dichloromethylene/hexane (1:1)