Dichloromethane → 4-Ethoxy-2'-hydroxy-3-thiophenecarboxanilide

HRID 236805

反応式

HRID 236805 の反応式
[CH2:1]([O:3][C:4]1[C:5]([C:9](Cl)=[O:10])=[CH:6][S:7][CH:8]=1)[CH3:2].C(Cl)Cl.N[O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C([N:25](CC)CC)C>O>[CH2:1]([O:3][C:4]1[C:5]([C:9]([NH:25][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[OH:16])=[O:10])=[CH:6][S:7][CH:8]=1)[CH3:2]

参加物

6

反応物 4

HCID 6344Dichloromethane2 回HCID 8471TriethylamineHCID 2794249O-PhenylhydroxylamineHCID 125737274-Ethoxy-3-thiophenecarbonyl chloride

生成物 1

HCID 125818594-Ethoxy-2'-hydroxy-3-thiophenecarboxanilide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 1.31 g. portion of 4-ethoxy-3-thiophenecarbonyl chloride is dissolved in 10 ml. of dry methylene chloride and then added dropwise to a solution of 0.75 g. of O-aminophenol in 10 ml. of dry methylene chloride with stirring. A 1.0 ml. portion of triethylamine is added and the mixture is then stirred overnight. This mixture is poured into water, stirred for 30 minutes and extracted three times with methylene chloride. The extracts are filtered through diatomaceous earth and then diluted with petroleum ether giving a white solid. This solid is recrystallized from a mixture of 250 ml. of methylene chloride and 250 ml. of petroleum ether giving 4-ethoxy-2'-hydroxy-3-thiophenecarboxanilide as white crystals.

後処理

  1. stirringstirred for 30 minutes
  2. extractionextracted three times with methylene chloride
  3. filtrationThe extracts are filtered through diatomaceous earth
  4. additiondiluted with petroleum ether giving a white solid
  5. customThis solid is recrystallized from a mixture of 250 ml

出典と根拠

ORDレコード
ord-2ecdd325b6a2492d8e01cdbe767c3661
出典データセット
uspto-grants-1979_06
特許番号
US04157444

関連ノート

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