Hydrochloric Acid → 6-Amino-5-chloro-3-methylbenzofuran

HRID 637689ノート

反応式

HRID 637689 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[Cl:13])[O:5][CH2:6][C:7](=O)[CH3:8].Cl>C(O)C>[NH2:1][C:2]1[C:12]([Cl:13])=[CH:11][C:10]2[C:7]([CH3:8])=[CH:6][O:5][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 202556581-(3-Amino-4-chlorophenoxy)-2-propanone

生成物 1

HCID 202556476-Amino-5-chloro-3-methylbenzofuran

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 11.4 g (57 mmole) of 1-(3-amino-4-chlorophenoxy)-2-propanone, 10 ml of concentrated hydrochloric acid and 150 ml of ethanol is boiled under reflux for 14 hours and subsequently concentrated by evaporation in vacuo. Ice-water is added to the residue and the whole is rendered alkaline with 3N sodium hydroxide solution and extracted with ether. The crude product obtained after drying and concentration by evaporation of the organic phase is chromatographed over silica gel with petroleum ether/methylene chloride. Recrystallisation of the pure fractions from ether/petroleum ether yields 6-amino-5-chloro-3-methylbenzofuran having a melting point of 73°-75°.

後処理

  1. temperatureunder reflux for 14 hours
  2. concentrationsubsequently concentrated by evaporation in vacuo
  3. additionIce-water is added to the residue
  4. extractionextracted with ether
  5. customThe crude product obtained
  6. customafter drying
  7. concentrationconcentration
  8. customby evaporation of the organic phase
  9. customis chromatographed over silica gel with petroleum ether/methylene chloride
  10. customRecrystallisation of the pure fractions from ether/petroleum ether

出典と根拠

ORDレコード
ord-37b17d8d4d044743838f4688dcbbaac8
出典データセット
uspto-grants-1985_12
特許番号
US04558043

反応ノート

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