反应详情

温度

210 °C

4,4′-methylene diphenyl dicarbamate (38 g, 86.8 mmole) and inhibitor benzoyl chloride (0.09 g, 0.6 mmole) were charged to 500 ml three-neck bottle containing solvent n-dodecane (250 ml, 191.4 g). The mixture was stirred with a magnetic stirbar and heated to 210° C. with an oil bath. One neck of the bottle was equipped with a thermometer and charged with nitrogen, and another neck was connected to a divide tube which was further connected to a condenser to charge with cold water. The upper end of the condenser was connected to a grease seal. The reaction was carried out for 2.5 hours. The progress of the reaction was monitored by FT-IR. It was observed that the absorption peak at 1720 cm−1 and the absorption peak at 3335 cm−1 disappeared completely, and an absorption peak appeared at 2270 cm−1. After part of n-dodecane (100 ml) and produced phenol (15.39 g) were retrieved from the divide tube, heating was stopped and the reaction ended.

1. customOne neck of the bottle was equipped with a thermometer
2. additioncharged with nitrogen, and another neck
3. customwas connected to a divide tube
4. customwhich was further connected to a condenser
5. customseal