Lawesson's reagent → 4-Methoxy-2'-methoxybenzothioanilide

HRID 1165478ノート

反応式

HRID 1165478 の反応式
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([C:7]([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])=O)=[CH:5][CH:4]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:29])=CC=1>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([C:7](=[S:29])[NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 3460502',4-Dimethoxybenzanilide

生成物 1

HCID 101073544-Methoxy-2'-methoxybenzothioanilide収率 153.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-Methoxy-2'-methoxybenzanilide (29.5 g) [Bull. Soc. Chim. France, 1964, (5), 924-935] was dissolved in 150 ml of toluene, and 25.6 g of Lawesson's reagent was added. The mixture was refluxed for 4.5 hours. After the reaction, the solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography [eluted with cyclohexane/ethyl acetate (7/1, v/v)] to give 26.5 g of 4-methoxy-2'-methoxybenzothioanilide.

後処理

  1. temperatureThe mixture was refluxed for 4.5 hours
  2. customAfter the reaction
  3. customthe solvent was evaporated under reduced pressure
  4. washeluted with cyclohexane/ethyl acetate (7/1

出典と根拠

ORDレコード
ord-94baf0ff19ed435c9ddb1361e448ac62
出典データセット
uspto-grants-1990_03
特許番号
US04910211

反応ノート

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