Phenol → 4-phenoxy-6-(1H-pyrazol-1-yl)pyrimidine

HRID 231804ノート

反応式

HRID 231804 の反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH:12]=[CH:11][CH:10]=[N:9]2)[CH:3]=1.[C:13]1([OH:19])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C1C=CC=CC=1>[O:19]([C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH:12]=[CH:11][CH:10]=[N:9]2)[CH:3]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 996PhenolHCID 106312394-Chloro-6-(1H-pyrazol-1-yl)pyrimidine

生成物 1

HCID 6613904-phenoxy-6-(1H-pyrazol-1-yl)pyrimidine

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

In 10 ml of benzene, 180 mg of 6-chloro-4-(1-pyrazolyl)pyrimidine, 175 ml of phenol, and 152 mg of 1,8-diazabicyclo-(5,4,0)-7-undecene (DBU) were dissolved, and refluxed for 7 hours. This reaction solution was washed with water, and an organic fraction was dried over anhydrous sodium sulfate. The resulting extract was distilled to give a residue, and the residue was purified by alumina gel column chromatography using a mixture of n-hexane and ethyl acetate (2:1) to yield 175 mg 6-phenoxy-4-(1-pyrazolyl)pyrimidine, recrystallized from n-hexane, to give an acicular crystal having a melting point of 92.5°-93.5° C.,

後処理

  1. temperaturerefluxed for 7 hours
  2. washThis reaction solution was washed with water
  3. dry with materialan organic fraction was dried over anhydrous sodium sulfate
  4. extractionThe resulting extract
  5. distillationwas distilled
  6. customto give a residue
  7. customthe residue was purified by alumina gel column chromatography
  8. additiona mixture of n-hexane and ethyl acetate (2:1)

出典と根拠

ORDレコード
ord-94235ced8b11461db88210b2fadce5e9
出典データセット
uspto-grants-1989_07
特許番号
US04849424

反応ノート

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