反应详情

To a solution of N-[1-(chloromethyl)-2-methylpropyl]-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-carboxamide(1.25 g, 2.63 mmol) in anhydrous tetrahydrofuran is added sodium hydride (60% oil dispersion, 0.116 g, 2.90 mmol). The resultant mixture is stirred 1.5 hour at room temperature, quenched with saturated ammonium chloride, diluted with diethyl ether, washed with saturated ammonium chloride and brine, and dried over anhydrous magnesium sulfate. Concentration in vacuo affords a yellow syrup, which is combined with material from a previous run and chromatographed on silica gel to afford the title compound as a white crystalline solid (mp 100-105° C.) which is identified by NMR spectral analysis.

1. customquenched with saturated ammonium chloride
2. additiondiluted with diethyl ether
3. washwashed with saturated ammonium chloride and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationConcentration in vacuo
6. customaffords a yellow syrup, which
7. customchromatographed on silica gel