Sodium Chloride → HCID 19045058, compound

Temperature

-78 °C

A solution of 2,2,3,3-tetrafluoro-2,3-dihydro-1,4-benzodioxin (5.00 g, 24.0 mmol) in dry tetrahydrofuran (150 mL) is cooled to -78° C. under a nitrogen atmosphere. A solution of n-butyllithium (10.6 mL, 26.4 mmol of a 2.5M solution in hexanes) is added dropwise while maintaining the reaction temperature below -65° C. The reaction mixture is stirred at -78° C. for 30 min and then 1,2-dibromotetrafluoroethane (3.16 mL, 26.4 mmol) is added dropwise. After this addition is complete, the reaction mixture is allowed to come to room temperature. A small mount of water is slowly added to the mixture which is then poured into water. The aqueous mixture is saturated with sodium chloride and is extracted with diethyl ether. The combined organic extracts are dried (MgSO4), filtered, and concentrated under reduced pressure to afford the title compound of Step A.

1. temperaturewhile maintaining the reaction temperature below -65° C
2. additionAfter this addition
3. customto come to room temperature
4. extractionis extracted with diethyl ether
5. dry with materialThe combined organic extracts are dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure

ORD record

ord-9130d3fad57549ea933b423cbc358a19

Source dataset

uspto-grants-1997_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05633218