3-(4-methoxy-3-methyl-phenyl)-1-methyl-1H-pyrazole → 2-methyl-4-(1-methyl-1H-pyrazol-3-yl)-phenol

HRID 628505ノート

反応式

HRID 628505 の反応式
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:13]=[CH:12][N:11]([CH3:14])[N:10]=2)=[CH:5][C:4]=1[CH3:15]>C(O)(=O)C>[CH3:15][C:4]1[CH:5]=[C:6]([C:9]2[CH:13]=[CH:12][N:11]([CH3:14])[N:10]=2)[CH:7]=[CH:8][C:3]=1[OH:2]

参加物

3

反応物 1

HCID 1182362533-(4-methoxy-3-methyl-phenyl)-1-methyl-1H-pyrazole

生成物 1

HCID 1367563942-methyl-4-(1-methyl-1H-pyrazol-3-yl)-phenol収率 90.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 3-(4-methoxy-3-methyl-phenyl)-1-methyl-1H-pyrazole 2.9 g, 47% hydrobromic acid 21 ml and acetic acid 21 ml was stirred with heating under reflux for twenty hours. The solvent was distilled off and to the resulting residues was added ethyl acetate 100 ml, and the resulting mixture was stirred at room temperature for one hour. The precipitates were filtered and were washed with hexane, and were concentrated under reduced pressure to give 2-methyl-4-(1-methyl-1H-pyrazol-3-yl)-phenol 2.45 g.

後処理

  1. temperaturewith heating
  2. temperatureunder reflux for twenty hours
  3. distillationThe solvent was distilled off and to the resulting residues
  4. additionwas added ethyl acetate 100 ml
  5. stirringthe resulting mixture was stirred at room temperature for one hour
  6. filtrationThe precipitates were filtered
  7. washwere washed with hexane
  8. concentrationwere concentrated under reduced pressure

出典と根拠

ORDレコード
ord-5f0ca30cd6794285852c9cbde3b852cd
出典データセット
uspto-grants-2016_04
特許番号
US09314023B2

反応ノート

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