Thionyl Chloride → 1-(Chloromethyl)-4-(ethylsulfonyl)benzene

HRID 271475

反応式

HRID 271475 の反応式
[CH2:1]([S:3]([C:6]1[CH:11]=[CH:10][C:9]([CH2:12]O)=[CH:8][CH:7]=1)(=[O:5])=[O:4])[CH3:2].S(Cl)([Cl:16])=O>ClCCl>[Cl:16][CH2:12][C:9]1[CH:10]=[CH:11][C:6]([S:3]([CH2:1][CH3:2])(=[O:5])=[O:4])=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 572424(4-(Ethylsulfonyl)phenyl)methanol

生成物 1

HCID 598347911-(Chloromethyl)-4-(ethylsulfonyl)benzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of (4-(ethylsulfonyl)phenyl)methanol (200 mg, 1 mmol) and thionyl chloride (3 mL) was stirred at reflux for 4 h. The solvent was removed under reduced pressure to obtain a gum. Dichloromethane (10 mL) was added, and the mixture was stirred for 5 min and then concentrated under vacuum. This process was repeated two more times to ensure complete removal of thionyl chloride. After residual solvent removal under vacuum, 205 mg of the title compound was obtained as a white solid. HPLC/MS: retention time=2.308 min, [M+H]+=219.

後処理

  1. temperatureat reflux for 4 h
  2. customThe solvent was removed under reduced pressure
  3. customto obtain a gum
  4. stirringthe mixture was stirred for 5 min
  5. concentrationconcentrated under vacuum
  6. customremoval of thionyl chloride
  7. customAfter residual solvent removal under vacuum

出典と根拠

ORDレコード
ord-da6685ace886414ead9b8f1d80fdfa93
出典データセット
uspto-grants-2008_11
特許番号
US07452892B2

関連ノート

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