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温度

0 °C

A 3-liter jacketed reactor vessel was charged with 100 ml of methylene chloride and cooled to approximately 0° C. A solution of 2-isopropenyl-2-oxazoline (100 g) in 177 ml of water, a solution of phosgene (131.5 g) in 400 ml of methylene chloride, and a solution of 35 weight percent sodium hydroxide in water were added simultaneously to the reaction vessel with stirring and cooling. The rates of addition were such that the three reagents were added over approximately a 50 minute time span with the temperature being maintained at 10° to 18° C. Stirring was continued for two minutes and the layers allowed to separate. The organic layer was washed twice with 100 ml portions of a saturated aqueous sodium bicarbonate solution, dried over sodium sulfate and concentrated under reduced pressure. The colorless concentrate was inhibited with 0.1 g of phenothiazine and the desired product recovered therefrom as a colorless liquid (133.6 g) boiling at 46°-47° C./0.4 mm Hg. Product yield 95-96 percent of theory.

1. temperaturecooling
2. additionThe rates of addition
3. additionwere added over approximately a 50 minute time span with the temperature
4. temperaturebeing maintained at 10° to 18° C
5. stirringStirring
6. customto separate
7. washThe organic layer was washed twice with 100 ml portions of a saturated aqueous sodium bicarbonate solution
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated under reduced pressure
10. concentrationThe colorless concentrate
11. customthe desired product recovered