反应详情

To methyl 6-(2,6-dichloro-4-(trifluoromethyl)phenyl)-4-methyl-1,2,6-thia-diazinan-2-carboxylate 1,1-dioxide (3.58 g, 8.50 mmol) in MeOH (60 mL), was dropwisely added 1 N NaOH (85 mL, 85 mmol) and agitated for 12 hr at room temperature. Following concentration under reduced pressure, ethyl acetate (30 mL) and water (30 mL) were added to the resultant to obtain the organic layer. The organic layer was dried over MgSO4 and crystallized using ethyl acetate (10 mL) and hexane (70 mL), giving the compound of interest (2.96 g, 96%, white solid). 1H NMR (300 MHz, CDCl3): δ 7.65 (s, 2H), 4.48-4.43 (m, 1H), 4.04-3.96 (m, 1H), 3.61-3.55 (m, 2H), 3.42-3.36 (m, 1H), 2.32 (m, 1H), 0.97 (d, 3H, J=6.8 Hz).

1. concentrationconcentration under reduced pressure, ethyl acetate (30 mL) and water (30 mL)
2. additionwere added to the resultant
3. customto obtain the organic layer
4. dry with materialThe organic layer was dried over MgSO4
5. customcrystallized
6. customgiving the compound of interest (2.96 g, 96%, white solid)