Acetic Acid → 2-(4-Methoxy-3,5-dimethylphenyl)-3-methylindole

HRID 2309403

反応式

HRID 2309403 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8](=O)[CH2:9][CH3:10])[CH:5]=[C:4]([CH3:12])[C:3]=1[O:13][CH3:14].[C:15]1([NH:21]N)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(O)(=O)C.Cl>C(O)C.O>[CH3:14][O:13][C:3]1[C:4]([CH3:12])=[CH:5][C:6]([C:8]2[NH:21][C:15]3[C:20]([C:9]=2[CH3:10])=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:7][C:2]=1[CH3:1]

参加物

7

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 7516PhenylhydrazineHCID 129634181-(4-Methoxy-3,5-dimethylphenyl)propan-1-one

生成物 1

HCID 136701412-(4-Methoxy-3,5-dimethylphenyl)-3-methylindole収率 62.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

5.0 g of 2,6-dimethyl-4-propionylanisole and 2.8 g of phenylhydrazine were dissolved in 30 ml of ethanol. A small amount of acetic acid was added under reflux for 30 minutes. After cooling, 10 ml of a 20% ethanol solution of hydrogen chloride was added to the reaction mixture, and the mixture was refluxed for 1.5 hours. The reaction mixture was cooled, poured into water, extracted with benzene, washed with water, and dried. The solvent was evaporated, and the residue was crystallized from benzene-hexane to give 4.3 g of 2-(4-methoxy-3,5-dimethylphenyl)-3-methylindole.

後処理

  1. temperatureunder reflux for 30 minutes
  2. temperatureAfter cooling
  3. temperaturethe mixture was refluxed for 1.5 hours
  4. temperatureThe reaction mixture was cooled
  5. extractionextracted with benzene
  6. washwashed with water
  7. customdried
  8. customThe solvent was evaporated
  9. customthe residue was crystallized from benzene-hexane

出典と根拠

ORDレコード
ord-5d813c2174c94bf3b27f28f1e5f7ede2
出典データセット
uspto-grants-1987_09
特許番号
US04695581

関連ノート

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