反应详情

In a round-bottomed flask was charged lithium aluminum hydride (3.8 g, 0.1 mole) in tetrahydrofuran (75 mL) and the contents was cooled in an ice-water bath at 0° to 5° C. 4,5-Dichloro-4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane (31.5 g, 0.1 mole) was added slowly. After the addition was complete, the reaction mixture was stirred at room temperature for 30 minutes. The resulting mixture was neutralized with 4.8N HCl (50 mL), then poured into 300 mL of ice-water. The bottom layer was separated and washed twice with cold water (200 mL). Distillation gave the saturated product 4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxolane (17 g, 69% yield) instead of the unsaturated dioxole product.

1. temperaturethe contents was cooled in an ice-water bath at 0° to 5° C
2. additionAfter the addition
3. customThe bottom layer was separated
4. washwashed twice with cold water (200 mL)
5. distillationDistillation