反应详情

温度

30 °C

Into a 5.0 L 4 necked RB flask, charged 100.0 g of 3-(4-nitro-1-oxo-1,3 dihydro-isoindol-2-yl)-piperidine-2,6-dione, 10.0 g of 10% Pd/C and 3200 ml of DMF under nitrogen atmosphere. Stirred the mass and raise the reaction mass temperature to 60 -65° C. Started the hydrogen gas bubbling into reaction mass at temperature 60-65° C. for 6 hours. The progress of the reaction is monitored by TLC. Cooled the mass to temperature 25to 30° C. Filtered the catalyst Pd/C under plant vacuum in the presence of nitrogen atmosphere and wash with dimethylformamide; wet Pd/C is transferred into a polythene bag for recovery. Distilled off the above organic layer solvent completely under vacuum below 60° C. Charged ethyl acetate 800 ml (lot-I) to the mass and stirred for 60 min. Filtered the solid and wash with 200 mL of ethyl acetate (Lot-II). Dried the above wet material in a oven at temperature 65-75° C. for 120-180 min. Dried Weight of the compound is 78.0 g.

1. temperatureraise the reaction mass temperature to 60 -65° C
2. custombubbling into reaction mass at temperature 60-65° C. for 6 hours
3. filtrationFiltered the catalyst Pd/C under plant vacuum in the presence of nitrogen atmosphere
4. washwash with dimethylformamide
5. distillationDistilled off the above organic layer solvent completely under vacuum below 60° C
6. stirringCharged ethyl acetate 800 ml (lot-I) to the mass and stirred for 60 min
7. filtrationFiltered the solid
8. washwash with 200 mL of ethyl acetate (Lot-II)
9. customDried the above wet material in a oven at temperature 65-75° C. for 120-180 min