反应详情

温度

110 °C

A 1 L three-necked flask, fitted with a stir bar and condenser, was charged with 3.0 g of HgO (yellow), 125 mL of 20% oleum, 25 mL of 65% oleum and 75.6 g of 3,4-dichloro-1-iodoperfluorobutane. After the reaction mixture was heated at 110° C. for 2 hours, the condenser was replaced by a distillation head with a 250 mL flask for receiver cooled with ice water. Volatiles were collected, washed with 98% sulfuric acid to remove sulfur trioxide and redistilled to give 40.3 g of 3,4-dichloroperfluorobutyryl fluoride, bp 72°-75° C., 99.8% GC purity.

1. customA 1 L three-necked flask, fitted with a stir bar and condenser
2. customthe condenser was replaced by a distillation head with a 250 mL flask for receiver
3. customVolatiles were collected
4. washwashed with 98% sulfuric acid
5. customto remove sulfur trioxide
6. distillationredistilled