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Hydrochloric Acid → HCID 86642965, 화합물

HRID 888642
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HRID 888642 반응식
C1(C)C=CC(S([O:10][CH2:11][CH2:12][C:13]([F:25])([F:24])[C:14]([F:23])([F:22])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17])(=O)=O)=CC=1.[C:27]([O-])(=[S:29])[CH3:28].[K+].Cl>CN(C)C=O>[C:27]([O:10][CH2:11][CH2:12][C:13]([F:24])([F:25])[C:14]([F:22])([F:23])[C:15]([F:20])([F:21])[C:16]([F:17])([F:18])[F:19])(=[S:29])[CH3:28]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 23670855Potassium ethanethioateHCID 866429663,3,4,4,5,5,6,6,6-Nonafluorohexyl 4-methylbenzene-1-sulfonate

생성물 1

HCID 86642965HCID 86642965, 화합물수율 57.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

A mixture of 42.65 g of 3,3,4,4,5,5,6,6,6-nonafluorohexyl p-toluenesulfonate, 100 ml of N,N-dimethylformamide and 11.65 g of potassium thioacetate was heated and stirred at 80° C. for 4 hours under a nitrogen atmosphere. A reaction vessel was cooled in an ice bath. To the reaction mixture was added an aqueous 1N hydrochloric acid solution, and the mixture was extracted with 200 ml of ethylacetate twice. Organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over sodium sulfate, filtered, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 18.91 g of 3,3,4,4,5,5,6,6,6-nonafluorohexyl thioacetate represented by the formula:

후처리

  1. temperaturewas heated
  2. temperatureA reaction vessel was cooled in an ice bath
  3. extractionthe mixture was extracted with 200 ml of ethylacetate twice
  4. washwashed with an aqueous saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-07e0b8b6ba364377a58e751349812a6d
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247596B2

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