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 is 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 is cooled to room temperature, diluted with 5 ml of chlorobenzene and washed with cold 5% aqueous sodium hydroxide and water. The organic phase is separated, dried over sodium sulfate, filtered and evaporated. The residue is 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. This material is triturated with ethyl acetate/hexane, filtered and dried to afford a solid, mp: 186-188° C.

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