Hydrochloric Acid → HCID 86612547, compound

Temperature

0 °C

1.6 g of 2-(3,3,3-trifluoropropyl)malononitrile was dissolved in 20 ml of a solution (1 mol/L) of tetrabutylammonium fluoride in tetrahydrofuran, 5 ml of 2-chloro-3,3,3-trifluoropropene was added thereto at 0° C., and the mixture was stirred at room temperature for 3 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 0.22 g of 2-(2-chloro-3,3,3-trifluoropropyl)-2-(3,3,3-trifluoropropyl)malononitrile (hereinafter, referred to as the present compound (58)).

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

ORD record

ord-a05ec5c8c1054e76b1009af982424a5b

Source dataset

uspto-grants-2010_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07662402B2