反应详情

温度

0 °C

9.93 g of 1'-cyano-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine] of Example 37 in 150 ml glyme and 100ml 6 M aqueous hydrochloric acid is heated at reflux under nitrogen for 1.5 hours. The mixture is cooled to 0° C., made basic with 50% aqueous sodium hydroxide (40 ml) and concentrated. The residue is dissolved in hot chloroform, washed with saturated sodium chloride, dried over anhydrous magnesium sulfate and contacted to give a crude product. Recrystallization from hot dimethylsulfoxide-dioxane-ether affords 1'-carbamoyl-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine], mp 217.5°-219.0° C.

1. temperatureat reflux under nitrogen for 1.5 hours
2. concentrationconcentrated
3. dissolutionThe residue is dissolved in hot chloroform
4. washwashed with saturated sodium chloride
5. dry with materialdried over anhydrous magnesium sulfate
6. customto give a crude product
7. customRecrystallization from hot dimethylsulfoxide-dioxane-ether