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

HRID 236805

반응식

HRID 236805 반응식
[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]

참가 물질

6

반응물 4

HCID 6344Dichloromethane2회HCID 8471TriethylamineHCID 2794249O-PhenylhydroxylamineHCID 125737274-Ethoxy-3-thiophenecarbonyl chloride

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2ecdd325b6a2492d8e01cdbe767c3661
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04157444

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