反应详情

温度

65 °C

To a solution of 2.3 g of 1-ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester in 26 ml of dimethylformamide is added 3 g of sodium methoxide. The reaction mixture is heated to 65° C. and stirred for 5 hours. The reaction mixture is poured into brine, neutralized and extracted with ethyl acetate. The organic phase is washed with brine, dried with sodium sulfate, filtered and concentrated. The residue is subjected to column chromatography (heptane/ethyl acetate 2:1) to yield 510 mg of 8-ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one as a solid, mp: >250° C.

1. extractionextracted with ethyl acetate
2. washThe organic phase is washed with brine
3. dry with materialdried with sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated