Thionyl Chloride → HCID 19934631、化合物

HRID 621633ノート

反応式

HRID 621633 の反応式
O[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:5]([O:16][CH3:17])[CH:4]=1.S(Cl)([Cl:20])=O>C(Cl)Cl>[Cl:20][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:5]([O:16][CH3:17])[CH:4]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 19934719HCID 19934719、化合物

生成物 1

HCID 19934631HCID 19934631、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The 1-hydroxymethyl-3-methoxy-4-phenylthiobenzene obtained above is dissolved in methylene chloride (372 ml), and thereto is added with strring thionyl chloride (9.12 ml) under ice cooling. The mixture is stirred for one hour, and the reaction mixture is washed with ice water (500 ml×2), and thereto is added ethyl acetate (500 ml). The mixture is washed in order with 5% aqueous sodium hydrogen carbonate solution (20 ml), water (200 ml) and saturated aqueous sodium chloride solution (200 ml×2), dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give 1-chloromethyl-3-methoxy-4-phenylthiobenzene.

後処理

  1. washthe reaction mixture is washed with ice water (500 ml×2)
  2. additionis added ethyl acetate (500 ml)
  3. washThe mixture is washed in order with 5% aqueous sodium hydrogen carbonate solution (20 ml), water (200 ml) and saturated aqueous sodium chloride solution (200 ml×2)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-77b86bc514ae4cf7a5fac992f70eaa65
出典データセット
uspto-grants-1989_04
特許番号
US04824834

反応ノート

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