Hydrochloric Acid → HCID 86612545, 화합물

HRID 1443559노트

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HRID 1443559 반응식
[C:1](#[N:5])[CH2:2][C:3]#[N:4].I[CH2:7][CH2:8][C:9]([F:18])([C:14]([F:17])([F:16])[F:15])[C:10]([F:13])([F:12])[F:11].C(=O)([O-])[O-].[K+].[K+].Cl>COCCOC>[F:18][C:9]([C:14]([F:17])([F:16])[F:15])([C:10]([F:13])([F:12])[F:11])[CH2:8][CH2:7][C:2]([CH2:7][CH2:8][C:9]([C:10]([F:11])([F:12])[F:13])([F:18])[C:14]([F:17])([F:16])[F:15])([C:1]#[N:5])[C:3]#[N:4]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8010MalononitrileHCID 11430Potassium CarbonateHCID 6296591,1,1,2-Tetrafluoro-4-iodo-2-(trifluoromethyl)butane

생성물 1

HCID 86612545HCID 86612545, 화합물수율 0.9%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

0.66 g of malononitrile and 9.7 g of 1-iodo-3,4,4,4-tetrafluoro-3-trifluoromethylbutane were dissolved in 10 ml of ethylene glycol dimethyl ether, 4.1 g of potassium carbonate was added, and the mixture was stirred at room temperature for 15 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 0.04 g of 2,2-bis(3,4,4,4-tetrafluoro-3-trifluoromethylbutyl)malononitrile (hereinafter, referred to as the present compound (56)).

후처리

  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

출처 및 근거

ORD 기록
ord-5903ff54f6da4f4ea6eae9fc3099a9d5
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662402B2

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