Methanesulfonyl chloride → 2-(3-Nitro-benzenesulfonyl)ethyl methanesulfonate

HRID 914995ノート

反応式

HRID 914995 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([S:10]([CH2:13][CH2:14][OH:15])(=[O:12])=[O:11])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[CH3:16][S:17](Cl)(=[O:19])=[O:18]>ClCCl.N1C=CC=CC=1>[CH3:16][S:17]([O:15][CH2:14][CH2:13][S:10]([C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)(=[O:12])=[O:11])(=[O:19])=[O:18]

参加物

5

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 170561Ethanol, 2-[(3-nitrophenyl)sulfonyl]-

生成物 1

HCID 589580692-(3-Nitro-benzenesulfonyl)ethyl methanesulfonate収率 71.5%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(3-nitrobenzenesulfonyl)ethanol (101) (5.0 g, 21.6 mmol) in dichloromethane (31.5 mL) and pyridine (7 mL) was added methanesulfonyl chloride (4.9 g, 43 mmol). The mixture was stirred at room temperature overnight before it was partitioned between dichloromethane (200 mL) and 0.5 N HCl (200 mL). The organic layer was dried over MgSO4 and concentrated on a rotavap to give 102 (4.78 g, 71%).

後処理

  1. customwas partitioned between dichloromethane (200 mL) and 0.5 N HCl (200 mL)
  2. dry with materialThe organic layer was dried over MgSO4
  3. concentrationconcentrated on a rotavap

出典と根拠

ORDレコード
ord-08464b2f7870468fa69c150e600cc333
出典データセット
uspto-grants-2007_09
特許番号
US07265122B2

反応ノート

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