反应详情

温度

90 °C

To a solution of 4-[4-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl)phenyl]piperazine-1-carboxylic acid benzyl ester (30 g) in 1,4-dioxane (450 ml) was added 1N-hydrochloric acid (240 ml) at ambient temperature, and the mixture was stirred for 7 hours at 90° C. The reaction mixture was poured into water. The mixture was adjusted to pH 10-12 with 1N-sodium hydroxide (480 ml), and extracted with ethyl acetate. The organic layer was washed with water, brine, and dried, and evaporated under reduced pressure. The residue was chromatographed on a column of silica gel eluting with dichloromethane/methyl alcohol (50:1) to give 4-[4-(4-oxopiperidin-1-yl)phenyl]piperazine-1-carboxylic acid benzyl ester (21.22 g).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water, brine
3. customdried
4. customevaporated under reduced pressure
5. customThe residue was chromatographed on a column of silica gel eluting with dichloromethane/methyl alcohol (50:1)