反应详情

Combine 30.0 gm. (0.16 M) N-(2,6-dimethylphenyl)-2-methylpropenamide [methacroyl-2',6'-xylidide], 13.3 gm. (0.16 M) lysidine, 3 gm. (0.03 M) methanesulphonic acid and 150 ml. of ethanol in a pressure bottle and heat at about 150° C. for about 48 hours. Remove the solvent in vacuo, add 200 ml. of water and adjust the pH to 7.8 with conc. HCl. Extract the aqueous phase with 4×100 ml. of methylene chloride and set these aside. Treat the aqueous phase with 20% NaOH to obtain a pH of about 13. Extract the aqueous phase with 4×100 ml. of methylene chloride. Wash the combined methylene chloride extracts with 3×10 ml. water and dry organic layer over sodium sulfate. Evaporate off the solvents to obtain the title compound.

1. customRemove the solvent in vacuo
2. additionadd 200 ml
3. extractionExtract the aqueous phase with 4×100 ml
4. additionTreat the aqueous phase with 20% NaOH
5. customto obtain a pH of about 13
6. extractionExtract the aqueous phase with 4×100 ml
7. washWash the combined methylene chloride
8. customEvaporate off the solvents