反应详情

β-Methallylsuccinic anhydride (539 g, 3.50 mole) was dissolved in toluene (800 mL) in a 1700 mL Parr stainless steel bottle fitted with a heating jacket. 10% Pd/C (3.60 g) was added and the bottle was connected to a Parr 2 L shaker fitted with two 4 L hydrogen tanks. After several evacuations and refilling with hydrogen, the shaker was started with the heater controlled for 60° C. The initial pressure was 60 lbs. When the pressure fell to 10 lbs, the tanks were repressurized to 60 lbs. After two hours, the controller was reset to 70° C. and the reaction was continued for another 12 hours. The heat was then turned off and after another 5 hours, the shaker was stopped. The reaction vessel was evacuated and the reaction mixture was filtered and concentrated. Distillation of the residue through the Vigreux column described above (P=9-10 mm Hg, T=180° C.) gave isobutylsuccinic anhydride (532.9 g, 97.6% yield).

1. customfitted with a heating jacket
2. customcontrolled for 60° C
3. customwas reset to 70° C.
4. waitthe reaction was continued for another 12 hours
5. waitThe heat was then turned off and after another 5 hours
6. customThe reaction vessel was evacuated
7. filtrationthe reaction mixture was filtered
8. concentrationconcentrated
9. distillationDistillation of the residue through the Vigreux column
10. customdescribed above (P=9-10 mm Hg, T=180° C.)