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

HRID 861836

反応式

HRID 861836 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
5 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-bfa83e74d423487693db90f92360767b
出典データセット
uspto-grants-1998_02
特許番号
US05716756

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