反应详情

Into 10 ml of tetrahydrofuran was dissolved 1.2 g of 3-hydroxy-5-(4-methanesulfonamidophenyl)-2-propionyl-2-cyclohexen-1-one and to the solution were added 0.6 g of methoxyamine hydrocholorate salt and 1.4 g of methanol containing 28% of sodium methylate. Then, the mixture was kept for 15 hours at room temperature and an insoluble material was filtered off from it and the resulting filtrate solution was concentrated under reduced pressure. Its residue was dissolved in chloroform and the solution was washed with a dilute hydrochloric acid solution and water, and it was dried with anhydrous magnesium sulfate. The chloroform was distilled off from it under a reduced pressure and ethyl ether was add in it. Thus, the crystal sedimented is collected with a filtering step and 1.2 g of the desired compound as colorless crystals having a melting point of 150°-151° C. was obtained.

1. filtrationan insoluble material was filtered off from it
2. concentrationthe resulting filtrate solution was concentrated under reduced pressure
3. dissolutionIts residue was dissolved in chloroform
4. washthe solution was washed with a dilute hydrochloric acid solution and water, and it
5. dry with materialwas dried with anhydrous magnesium sulfate
6. distillationThe chloroform was distilled off from it under a reduced pressure and ethyl ether
7. additionwas add in it
8. customThus, the crystal sedimented is collected with a filtering step and 1.2 g of the desired compound as colorless crystals
9. customwas obtained