Methanesulfonyl chloride → [4-chloro-2-(1-chloroethyl)phenoxy]-acetic Acid, 1,1-dimethylethyl Ester

HRID 38260ノート

反応式

HRID 38260 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][CH2:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[C:4]([CH:17](O)[CH3:18])[CH:3]=1.CCN(C(C)C)C(C)C.CS([Cl:33])(=O)=O>C(Cl)Cl>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][CH2:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[C:4]([CH:17]([Cl:33])[CH3:18])[CH:3]=1

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 86631057[4-chloro-2-(1-hydroxyethyl)phenoxy]-acetic Acid, 1,1-dimethylethyl Ester

生成物 1

HCID 86631056[4-chloro-2-(1-chloroethyl)phenoxy]-acetic Acid, 1,1-dimethylethyl Ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To the product of step b) (0.34 g) in DCM (5 ml) was added Hunigs base (1 ml) followed by methanesulfonyl chloride (0.46 ml) and the reaction stirred at room temperature for 2 h followed by heating at 45° C. for 2 h. After cooling to 0° C. the bulk of the volatiles were removed in vacuo. Diethyl ether and water were added and the organic layer separated.

後処理

  1. temperatureby heating at 45° C. for 2 h
  2. temperatureAfter cooling to 0° C. the bulk of the volatiles
  3. customwere removed in vacuo
  4. additionDiethyl ether and water were added
  5. customthe organic layer separated

出典と根拠

ORDレコード
ord-751bf4b766aa40ed99c35ebfb6283106
出典データセット
uspto-grants-2013_09
特許番号
US08524715B2

反応ノート

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