4-(5-Trifluoromethyl-pyridin-2-yloxy)-phenol → 2-Hydroxyphenoxy-5-trifluoromethyl pyridine

HRID 1980405

反応式

HRID 1980405 の反応式
CO[C:3]1[CH:19]=[CH:18][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][N:9]=2)=[CH:5][CH:4]=1.[OH:20]C1C=CC(OC2C=CC(C(F)(F)F)=CN=2)=CC=1>C(O)(=O)C.Br>[OH:20][C:18]1[CH:19]=[CH:3][CH:4]=[CH:5][C:6]=1[O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][N:9]=1

参加物

5

反応物 2

HCID 1552414-(5-Trifluoromethyl-pyridin-2-yloxy)-phenolHCID 155242Pyridine, 2-(4-methoxyphenoxy)-5-(trifluoromethyl)-

生成物 1

HCID 204028222-Hydroxyphenoxy-5-trifluoromethyl pyridine

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 260Hydrogen Bromide溶媒

実験手順

2-p-Methoxyphenoxy-5-trifluoromethylpyridine (10.5 g) in glacial acetic acid (100 ml) and 48% hydrobromic acid (50 ml) were stirred and heated under reflux for 71/2 hours. The solution was then evaporated and the remaining oil treated with sodium bicarbonate solution and shaken with ether (2×300 ml). The ether extract was shaken with 2-molar sodium hydroxide solution (200 ml) and then water (150 ml). The aqueous layers were combined, acidified with 2-molar hydrochloric acid and extracted with ether (2×300 ml). The ether extract was dried and evaporated to give a brown oil identified as 2-p-hydroxyphenoxy-5-trifluoromethylpyridine.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 71/2 hours
  3. customThe solution was then evaporated
  4. additionthe remaining oil treated with sodium bicarbonate solution
  5. extractionThe ether extract
  6. stirringwas shaken with 2-molar sodium hydroxide solution (200 ml)
  7. extractionextracted with ether (2×300 ml)
  8. extractionThe ether extract
  9. customwas dried
  10. customevaporated
  11. customto give a brown oil

出典と根拠

ORDレコード
ord-748fdbcf9734406080217112f92e468b
出典データセット
uspto-grants-1985_04
特許番号
US04508907

関連ノート

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