反应详情

温度

50 °C

To a solution of 200 mg of 3-(2,5-dimethyl-phenyl)-4-hydroxy-8-methoxy-1,8-diaza-spiro[4.5]dec-3-en-2-one and 0.14 ml of ethyl diisopropyl amine in 2 ml of chlorobenzene was added a solution of 66 mg of methyl chloroformate in 0.5 ml of chlorobenzene at 50° C. After stirring for 1 hour at 50° C., the reaction mixture was cooled to room temperature, diluted with 5 ml of chlorobenzene and washed with cold 5% aqueous sodium hydroxide and water. The organic phase was separated, dried over sodium sulfate, filtered and evaporated. The residue was purified by flash chromatography on silica gel. Yield: 120 mg of carbonic acid 3-(2,5-dimethyl-phenyl)-8-methoxy-2-oxo-1,8-diaza-spiro[4.5]dec-3-en-4-yl ester methyl ester (title compound A1). This material was triturated with ethyl acetate/hexane, filtered and dried to afford a solid, mp: 186-188° C.

1. temperaturethe reaction mixture was cooled to room temperature
2. washwashed with cold 5% aqueous sodium hydroxide and water
3. customThe organic phase was separated
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by flash chromatography on silica gel
8. customThis material was triturated with ethyl acetate/hexane
9. filtrationfiltered
10. customdried
11. customto afford a solid, mp: 186-188° C.