Hydrochloric Acid → HCID 15979662, compound

Temperature

60 °C

2.0 g of 2-(3,3,3-trifluoropropyl)malononitrile and 4.7 g of 2,2,3,3,4,4,5,5,5-nonafluoropentyl trifluoromethanesulfonate were dissolved in 10 ml of N,N-dimethylformamide, 2.0 g of potassium carbonate was added, and the mixture was stirred at 60° C. for 4 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with methyl tert-butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate 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 to obtain 0.87 g of 2-(2,2,3,3,4,4,5,5,5-nonafluoropentyl)-2-(3,3,3-trifluoropropyl)malononitrile (hereinafter, referred to as the present compound (5.3)).

1. extractionfollowed by extraction with methyl tert-butyl ether
2. washThe organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure

ORD record

ord-32982038ef9f41998c7515376c238665

Source dataset

uspto-grants-2010_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07662402B2