Hydrochloric Acid → 2,2-Bis(2,2,3,4,4,4-hexafluorobutyl)malononitrile
반응식
[F:1][C:2]([F:15])([CH:9]([F:14])[C:10]([F:13])([F:12])[F:11])[CH2:3][CH:4]([C:7]#[N:8])[C:5]#[N:6].FC(F)(F)S(O[CH2:22][C:23]([F:31])([F:30])[CH:24]([F:29])[C:25]([F:28])([F:27])[F:26])(=O)=O.C(=O)([O-])[O-].[K+].[K+].Cl>CC(C)=O>[F:1][C:2]([F:15])([CH:9]([F:14])[C:10]([F:12])([F:13])[F:11])[CH2:3][C:4]([CH2:22][C:23]([F:31])([F:30])[CH:24]([F:29])[C:25]([F:28])([F:27])[F:26])([C:7]#[N:8])[C:5]#[N:6]참가 물질
실험 절차
In 50 ml of acetone, 2.0 g of 2-(2,2,3,4,4,4-hexafluorobutyl)malononitrile and 5.3 g of 2,2,3,4,4,4-hexafluorobutyl trifluoromethanesulfonate were dissolved, 1.9 g of potassium carbonate was added and the mixture was stirred at room temperature for 10 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture and the mixture was extracted with t-butyl methyl 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 0.05 g of 2,2-bis(2,2,3,4,4,4-hexafluorobutyl)malononitrile (hereinafter, referred to as the present compound (95)).
후처리
- extractionthe mixture was extracted with t-butyl methyl ether
- washThe organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-1345aecfa3a44cb683da51e10c225436
- 출처 데이터셋
- uspto-grants-2010_02
- 특허 번호
- US07662402B2
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