Triethylamine → 2-Methanesulfonyloxy-2-p-tolyl-1,1,1,3,3,3-hexafluoropropane

HRID 861836

반응식

HRID 861836 반응식
[F:1][C:2]([F:17])([F:16])[C:3]([C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)([OH:8])[C:4]([F:7])([F:6])[F:5].C(N(CC)CC)C.[CH3:25][S:26](Cl)(=[O:28])=[O:27]>C(Cl)Cl>[CH3:25][S:26]([O:8][C:3]([C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)([C:4]([F:6])([F:5])[F:7])[C:2]([F:16])([F:17])[F:1])(=[O:28])=[O:27]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 748292-(p-Tolyl)hexafluoroisopropanol

생성물 1

HCID 197002732-Methanesulfonyloxy-2-p-tolyl-1,1,1,3,3,3-hexafluoropropane수율 71.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
5 °C

실험 절차

5.16 g (20 mmol) of 1,1,1,3,3,3-hexafluoro-2-p-tolylpropan-2-ol were dissolved in 50 ml of methylene chloride, and 2.8 g (28 mmol) of triethylamine were added. 3.2 g (22 mmol) of methanesulfonyl chloride were added dropwise, while stirring, to the solution cooled to 5° C. After warming up to room temperature, the mixture was allowed to stand overnight. The precipitated salt was filtered off and the organic solution was evaporated down. The subsequent chromatography (silica gel/methylene chloride) gave 4.8 g of 2-methanesulfonyloxy-2-p-tolyl-1,1,1,3,3,3-hexafluoropropane (pale yellow oil).

후처리

  1. temperatureAfter warming up to room temperature
  2. filtrationThe precipitated salt was filtered off
  3. customthe organic solution was evaporated down

출처 및 근거

ORD 기록
ord-bfa83e74d423487693db90f92360767b
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05716756

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