反应详情

温度

90 °C

A mixture of 8-(2-chloro-pyridine-3-sulfonyl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one (described in example 188, 40 mg, 0.08 mmol) and 8M methyl amine solution in ethanol (408 uL, 3.26 mmol) and was heated to 90° C. in a sealed tube for 48 h. The reaction mixture was transferred to a round bottom flask and concentrated in vacuo to give a crude residue which was diluted with ethyl acetate and washed with water, sat. NaHCO3 and brine. The organic layer was dried (Na2SO4), filtered and evaporated under reduced pressure to give a crude residue which was purified by flash column chromatography using Amine-Silica to yield the desired product as a white solid (39 mg, 98%). MS (ESI): 485.2 (MH+).

1. customThe reaction mixture was transferred to a round bottom flask
2. concentrationconcentrated in vacuo
3. customto give a crude residue which
4. washwashed with water, sat. NaHCO3 and brine
5. dry with materialThe organic layer was dried (Na2SO4)
6. filtrationfiltered
7. customevaporated under reduced pressure
8. customto give a crude residue which
9. customwas purified by flash column chromatography