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Dichloromethane → (3,3-difluorocyclobutyl)methyl methanesulfonate

HRID 1844173
ノート
印刷プレビュー

反応式

HRID 1844173 の反応式
[F:1][C:2]1([F:8])[CH2:5][CH:4]([CH2:6][OH:7])[CH2:3]1.ClCCl.C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>O>[CH3:19][S:20]([O:7][CH2:6][CH:4]1[CH2:5][C:2]([F:8])([F:1])[CH2:3]1)(=[O:22])=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 45480377(3,3-Difluorocyclobutyl)methanol

生成物 1

HCID 58223412(3,3-difluorocyclobutyl)methyl methanesulfonate収率 107%

試薬・触媒・溶媒 1

HCID 962Water溶媒
このページの内容参加物実験手順後処理出典と根拠反応ノート

実験手順

1.35 g (11.06 mmol) of (3,3-difluorocyclobutyl)methanol were initially charged in 41.8 ml of abs. dichloromethane, 3.08 ml (22.11 mmol) of triethylamine and 1.03 ml (13.27 mmol) of methanesulphonyl chloride were added and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture and the aqueous phase was extracted twice with dichloromethane. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and filtered, and the filtrate was concentrated. This gave 2.37 g (quantitative yield) of the target compound.

後処理

  1. extractionthe aqueous phase was extracted twice with dichloromethane
  2. washThe combined organic phases were washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-0415840638ca43a9a7ea8438ddec31b6
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946215B2

反応ノート

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