反应详情

温度

60 °C

A mixture of (R)-8-(5-bromo-2-fluoro-phenyl)-8-methyl-6,6-dioxo-6λ6-thia-9-aza-spiro[4.5]dec-2-en-10-thione (300 mg, 742 μmol, Eq: 1.00) and ammonia (7 N in MeOH) (7.87 g, 10 ml, 70.0 mmol, Eq: 94.3) was stirred in a sealed tube for 48 hours at 60° C. Extracted with ethyl acetate and sat. NaHCO3-sol., dried the organic layer over Na2SO4, filtered and evaporated. The residue was chromatographed with ethyl acetate to give (R)-8-(5-bromo-2-fluoro-phenyl)-8-methyl-6,6-dioxo-6λ6-thia-9-aza-spiro[4.5]deca-2,9-dien-10-ylamine (249 mg, 643 μmol, 86.7% yield) as a white foam. MS (ISP): m/z=387.3 [M+H]+ and 389.3 [M+2+H]+.

1. extractionExtracted with ethyl acetate and sat. NaHCO3-sol
2. dry with material, dried the organic layer over Na2SO4
3. filtrationfiltered
4. customevaporated
5. customThe residue was chromatographed with ethyl acetate