反应详情

Four hundred seventy four grams (3.0 moles) of isodecyl alcohol, 750 g (7.5 moles) of methyl methacrylate (MMA), 1.75 g (3.0 millimol) of hafnium actylacetonate, and 50 mg diethylhydroxylamine and 25 mg phenothiazine free radical polymerization inhibitors, are added to a 3 liter flask equipped with an agitator, thermometer, and a 10-plate Oldershaw fractional distillation column. The mixture was heated to reflux at atmospheric pressure while an azeotropic mixture of MMA and methanol was removed from the upper part of the fractionating column. The reaction was continued in this manner for approximately 90 minutes while the temperature at the top of the column was 65°-67° C. and the temperature in the pot was 106°-124° C. Excess MMA was removed under vacuum and the resulting IDMA was isolated (660 grams, 99.0% yield) and analyzed. Gas-liquid chromatographic (GLC) analysis showed >99.9% conversion of isodecanol to IDMA of 99.8% purity.

1. additionare added to a 3 liter flask
2. customequipped with an agitator
3. distillationthermometer, and a 10-plate Oldershaw fractional distillation column
4. temperatureThe mixture was heated
5. temperatureto reflux at atmospheric pressure while an azeotropic mixture of MMA and methanol
6. customwas removed from the upper part of the fractionating column
7. customwas 65°-67° C.
8. custompot was 106°-124° C
9. customExcess MMA was removed under vacuum
10. customthe resulting IDMA was isolated (660 grams, 99.0% yield)