反应详情

温度

15 °C

A solution of 3.88 g of methanesulfonyl chloride is added at 0° C. to a suspension of 8.5 g of the product obtained in Stage A in 100 ml of tetrahydrofuran. The mixture is left stirring for 3 hours at 15° C., and this suspension is then added to a solution, cooled to 0° C., of 4.4 g of ethyl acetoacetate containing 1.63 g of sodium hydride in 100 ml of tetrahydrofuran. The mixture is then brought to reflux for 12 hours, hydrolyzed with 5 ml of water and concentrated, and the residue is take up in 150 ml of dichloromethane. The organic phase is washed with 50 ml of water, dried over anhydrous sodium sulfate and concentrated. The oil obtained is purified by chromatography on 600 g of 70-230 mesh silica, using a mixture of dichloromethane and methanol (99:1 V/V) as eluant.

1. waitThe mixture is left
2. additionthis suspension is then added to a solution
3. concentrationconcentrated
4. washThe organic phase is washed with 50 ml of water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe oil obtained
8. customis purified by chromatography on 600 g of 70-230 mesh silica
9. additiona mixture of dichloromethane and methanol (99:1 V/V) as eluant