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Methanesulfonyl chloride → 2-(Methylsulfonyl)ethyl methanesulfonate

HRID 627025
ノート
印刷プレビュー

反応式

HRID 627025 の反応式
[CH3:1][S:2]([CH2:5][CH2:6][OH:7])(=[O:4])=[O:3].C(N(C(C)C)CC)(C)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>C(Cl)Cl>[CH3:17][S:18]([O:7][CH2:6][CH2:5][S:2]([CH3:1])(=[O:4])=[O:3])(=[O:20])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 848342-(Methylsulfonyl)ethanol

生成物 1

HCID 184645972-(Methylsulfonyl)ethyl methanesulfonate収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a 50 mL round-bottomed flask, 2-(methylsulfonyl)ethanol (1.24 g, 9.99 mmol, Eq: 1.00) was combined with DCM (5 mL). To the resulting solution was added diisopropylethylamine (2.1 mL, 12.0 mmol, Eq: 1.2) and methanesulfonyl chloride (1.37 g, 931 μL, 12.0 mmol, Eq: 1.2). The ice bath was removed and the reaction was stirred at rt overnight. The crude reaction mixture was concentrated in vacuo and the residue was partitioned between EtOAc and water. The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 80 g, 10% to 80% EtOAc in hexanes) to give 2-(methylsulfonyl)ethyl methanesulfonate (1.01 g).

後処理

  1. customThe ice bath was removed
  2. customThe crude reaction mixture
  3. concentrationwas concentrated in vacuo
  4. customthe residue was partitioned between EtOAc and water
  5. dry with materialThe organic layer was dried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe crude material was purified by flash chromatography (silica gel, 80 g, 10% to 80% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-59af46faaf0f486bb3881a064cbe3f58
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309248B2

反応ノート

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