Water → Cyclopropanemethanol, 2,2-difluoro-, 1-methanesulfonate

HRID 1026326ノート

反応式

HRID 1026326 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[F:6][C:7]1([F:12])[CH2:9][CH:8]1[CH2:10][OH:11].C(N(CC)CC)C.O>C1COCC1>[CH3:1][S:2]([O:11][CH2:10][CH:8]1[CH2:9][C:7]1([F:12])[F:6])(=[O:4])=[O:3]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 2761401(2,2-Difluorocyclopropyl)methanol

生成物 1

HCID 58198163Cyclopropanemethanol, 2,2-difluoro-, 1-methanesulfonate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Methanesulfonyl chloride (1.43 mL) was added to a solution of (2,2-difluorocyclopropyl)methanol (1.00 g) and triethylamine (2.58 mL) in THF (10 mL) dropwise at 0° C. The mixture was stirred at room temperature overnight. Water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (1.47 g) as a colorless oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-8b19d6c282684771ab89f3e86b77613a
出典データセット
uspto-grants-2014_05
特許番号
US08729102B2

反応ノート

読み込み中…