Water → HCID 86612540, compound

7.5 g of malononitrile was dissolved in 50 ml of N,N-dimethylformamide and 10.4 g of potassium carbonate was added. The mixture was stirred at room temperature for 1 hour, 10.0 g of 2,2,3,3-tetrafluoropropyl trifluoromethanesulfonate dissolved in 20 ml of N,N-dimethylformamide was added dropwise, and the mixture was stirred overnight. Thereafter, the reaction mixture was poured to water and extracted with diethyl ether. The organic layer was washed successively with water and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography. The resulting fraction was washed with chloroform to obtain 0.08 g of 2,2-bis(2,2,3,3-tetrafluoropropyl)malononitrile (hereinafter, referred to as the present compound (50)).

1. additionwas added dropwise
2. stirringthe mixture was stirred overnight
3. extractionextracted with diethyl ether
4. washThe organic layer was washed successively with water and aqueous saturated sodium chloride
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. washThe resulting fraction was washed with chloroform

ORD record

ord-12aa6b6bc3774a4592777a90c8b28b4c

Source dataset

uspto-grants-2010_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07662402B2