Oxygen → Tetrahydrophthalic anhydride
반응식
[CH2:1]=[CH:2]/[CH:3]=[CH:4]/C.[C:6]1(=[O:12])[O:11][C:9](=[O:10])[CH:8]=[CH:7]1.C(C1C=C(O)C(=CC=1)O)(C)(C)C.S(CCC(OCCCCCCCCCCCC)=O)CCC(OCCCCCCCCCCCC)=O.O=O>>[CH2:1]1[CH:7]2[C:6]([O:11][C:9](=[O:10])[CH:8]2[CH2:4][CH:3]=[CH:2]1)=[O:12]참가 물질
6
실험 절차
3Me--THPA was produced by the gas phase aeration method. Thus, the air in a 300-ml four-necked flask equipped with a stirrer, thermometer, condenser, a dropping funnel for feeding crude trans-1,3-pentadiene, and an unreactive fraction recovery vessel was replaced with nitrogen and, then, the flask was charged with 98 g of maleic anhydride, 500 ppm of p-tert-butylcatechol by way of radical polymerization inhibitor and 1000 ppm of dilauryl thiodipropionate as auxiliary polymerization inhibitor. The charge was melted at 50° to 55° C. and after the internal atmosphere was replaced with nitrogen gas, nitrogen gas containing 4% of oxygen was passed through the gas phase at a rate of 10 ml/min throughout the reaction period. Under this atmosphere, 374 g of crude trans-1,3-pentadiene of the same composition as that used in Example 1 was continuously added at 50° to 55° C. over a period of 4 hours. During the reaction, major portion of unreactive fractions was distilled off from the reaction system. After completion of addition, the reaction was conducted at 70° C. for 30 minutes. After completion of the reaction, the reaction mixture was distilled at 85° C. under atmospheric pressure and, then, under reduced pressure to remove the volatile fraction. In this manner, 164 g of 3Me--THPA was obtained. The investigation revealed no gels in the product.