Dichloromethane → 5'-Chloro-4-ethoxy-2'-hydroxy-3-thiophenecarboxanilide

HRID 614210ノート

反応式

HRID 614210 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.[Cl:15][C:16]1[CH:17]=[CH:18][C:19]([OH:23])=[C:20]([CH:22]=1)[NH2:21]>C(N(CC)CC)C>[Cl:15][C:16]1[CH:17]=[CH:18][C:19]([OH:23])=[C:20]([CH:22]=1)[NH:21][C:9]([C:5]1[C:4]([O:3][CH2:1][CH3:2])=[CH:8][S:7][CH:6]=1)=[O:10]

参加物

5

反応物 3

HCID 6344Dichloromethane2 回HCID 72652-Amino-4-chlorophenolHCID 125737274-Ethoxy-3-thiophenecarbonyl chloride

生成物 1

HCID 213159805'-Chloro-4-ethoxy-2'-hydroxy-3-thiophenecarboxanilide

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

An 8.8 g. portion of 4-ethoxy-3-thiophenecarbonyl chloride is dissolved in 100 ml. of methylene chloride and added dropwise to a mixture of 6.6 g. of 5-chloro-2-hydroxyaniline in 100 ml. of methylene chloride and 6.5 ml. of triethylamine. This mixture is stirred at ambient temperature overnight, concentrated to 100 ml. and filtered. The filtrate is allowed to stand overnight and the precipitate which forms is collected, washed with water and dried in vacuo. This combined precipitate is recrystallized from 200 ml. of ethanol, treated with charcoal, filtered through diatomaceous earth and concentrated giving 5'-chloro-4-ethoxy-2'-hydroxy-3-thiophenecarboxanilide as red brown crystals.

後処理

  1. concentrationconcentrated to 100 ml
  2. filtrationand filtered
  3. waitto stand overnight
  4. customthe precipitate which forms is collected
  5. washwashed with water
  6. customdried in vacuo
  7. customThis combined precipitate is recrystallized from 200 ml
  8. additionof ethanol, treated with charcoal
  9. filtrationfiltered through diatomaceous earth
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-862aea1c7d194c82b153557f6da43e53
出典データセット
uspto-grants-1979_03
特許番号
US04144235

反応ノート

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