Chlorosulfonic acid → [2-(4-Fluorophenoxy)phenyl]sulfonyl chloride

HRID 2265876ノート

反応式

HRID 2265876 の反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:19]=[CH:18][C:10]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:9][CH:8]=1>ClCCl>[F:6][C:7]1[CH:19]=[CH:18][C:10]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[S:2]([Cl:1])(=[O:5])=[O:3])=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 676141-Fluoro-4-phenoxybenzene

生成物 1

HCID 5187142[2-(4-Fluorophenoxy)phenyl]sulfonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

16.1 g (0.138 mol) of chlorosulfonic acid are slowly added dropwise to a solution of 13.05 g of 4-fluorophenoxybenzene (0.069 mol) cooled to 0° C. After the addition is complete, the mixture is stirred at room temperature for a further 4 hours. For work up, 50 ml of dichloromethane are added, and the mixture is washed once with H2O. The aqueous phase is separated off and extracted twice more with 50 ml of dichloromethane each time. The combined organic phases are dried with MgSO4 and concentrated, resulting in the title compound as a colorless solid. Yield: 11.03 g; 60%.

後処理

  1. additionAfter the addition
  2. washthe mixture is washed once with H2O
  3. customThe aqueous phase is separated off
  4. extractionextracted twice more with 50 ml of dichloromethane each time
  5. dry with materialThe combined organic phases are dried with MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-eb20f46957c549419a0abe64f464ee33
出典データセット
uspto-grants-2010_12
特許番号
US07858619B2

反応ノート

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