反应详情

To a solution of 7-acetyl-4-hydroxy-1,3-benzothiazol-2(3H)-one (153 mg), in dry THF (3 ml) and dry DMF (0.5 ml) under nitrogen, was added N,N-diisopropylethylamine (0.13 ml) and benzyl bromide (0.09 ml), and the mixture stirred for 72 h. Water (10 ml) was added and the mixture extracted with ethyl acetate. The organic phases were combined, washed with brine, dried (MgSO4), and evaporated in vacuo. The residue was purified on a 5 g silica SPE cartridge, eluting with a stepped gradient of 10% to 50% ethyl acetate-cyclohexane mixtures, to give the title compound (68 mg). LCMS RT=3.14 min.

1. extractionthe mixture extracted with ethyl acetate
2. washwashed with brine
3. dry with materialdried (MgSO4)
4. customevaporated in vacuo
5. customThe residue was purified on a 5 g silica SPE cartridge
6. washeluting with a stepped gradient of 10% to 50% ethyl acetate-cyclohexane mixtures