反应详情

温度

50 °C

A stirred mixture of 14 g of the product of Step A, 140 ml of acetic acid and 1.4 g of 9.6% palladized carbon was heated at 50° C. while saturated with hydrogen and when hydrogen absorption ceased, the mixture was filtered. The filtrate was evaporated to dryness and the residue was taken up in water. The aqueous phase was made alkaline with sodium hydroxide and the mixture was extracted with methylene chloride. The organic phase was washed with water, dried and evaporated to dryness to obtain 8.5 g of raw product. The latter was chromatographed over silica gel and was eluted with an 85-10-5 chloroform-methanol-triethylamine mixture to obtain 1,3-dihydro-5-methoxy-3-(piperidin-4-yl)-2H-indol-2-one with a Rf=0.15.

1. customsaturated with hydrogen and when hydrogen absorption
2. filtrationthe mixture was filtered
3. customThe filtrate was evaporated to dryness
4. extractionthe mixture was extracted with methylene chloride
5. washThe organic phase was washed with water
6. customdried
7. customevaporated to dryness
8. customto obtain 8.5 g of raw product
9. customThe latter was chromatographed over silica gel
10. washwas eluted with an 85-10-5 chloroform-methanol-triethylamine mixture