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

HRID 628505노트

반응식

HRID 628505 반응식
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]

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5f0ca30cd6794285852c9cbde3b852cd
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09314023B2

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