反应详情

2,2,2-trifluoroethanol (105 g 1.05 mol), pyridine (87 g 1.1 mol) and 300 mL of methylene chloride were combined in a 1 L 3-neck round bottom flask. The flask was equipped with an overhead stirring mechanism, thermocouple, addition funnel, cold water condenser, and a dry nitrogen bubbler. The reaction flask was kept cool using a dry ice/acetone bath to keep the temperature in the range of −20° C. to −15° C. Methylchloroformate (100 g 1.05 mol) was added via an addition funnel at such a rate that the temperature was kept in the range of −20° C. to −15° C. Once the addition of the methylchloroformate was complete the reaction mix was allowed to warm to room temperature. The reaction mix was then quenched with 100 mL water. The methylene chloride solution was separated from the water and washed with 2×100 mL of 1N HCl. The methylene chloride was removed by distillation and the product was purified using fractional distillation on a concentric tube column (b.p.=90.0° C., purity=99.7%). The structure mass was confirmed by GC/MS.

1. customThe flask was equipped with an overhead
2. additionthermocouple, addition funnel, cold water condenser
3. temperatureThe reaction flask was kept cool
4. customin the range of −20° C. to −15° C
5. customwas kept in the range of −20° C. to −15° C
6. additionmix
7. additionThe reaction mix
8. customwas then quenched with 100 mL water
9. customThe methylene chloride solution was separated from the water
10. washwashed with 2×100 mL of 1N HCl
11. customThe methylene chloride was removed by distillation
12. customthe product was purified
13. distillationdistillation on a concentric tube column (b.p.=90.0° C., purity=99.7%)