4-Cyanophenol → Isopropyl alcohol isopropyl ether

HRID 261070

反応式

HRID 261070 の反応式
S1C2CN[CH2:8][CH2:9][C:4]=2C=C1.C(C1C=[CH:16][C:15]([OH:18])=[CH:14]C=1)#N>O1CCOCC1>[CH:15]([O:18][CH:9]([CH3:8])[CH3:4])([CH3:16])[CH3:14].[CH:15]([OH:18])([CH3:16])[CH3:14]

参加物

5

反応物 3

HCID 130194-CyanophenolHCID 123370254H,5H,6H,7H-thieno(2,3-c)pyridineHCID 178486302HCID 178486302、化合物

生成物 1

HCID 21202047Isopropyl alcohol isopropyl ether収率 23%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4,5,6,7-tetrahydro-thieno[2,3-c]pyridine (1 g; 7.2 mmoles), p-cyano-phenol (95% purity; 0.9 g; 7.2 mmoles), polyoxymethylene (0.43 g; 14.4 mmoles) and dioxan (20 cc) is stirred at 80° C. during 4 hours. After concentration in vacuo, the residue is taken up into 2N hydrochloric acid. The aqueous phase is extracted with ether, made basic with concentrated ammonia and again extracted with methylene chloride. The organic extracts are washed with water, dried over sodium sulfate and concentrated in vacuo. The residue is recrystallized from isopropyl ether-isopropanol (M.p. 134° C.; yield: 23%).

後処理

  1. concentrationAfter concentration in vacuo
  2. extractionThe aqueous phase is extracted with ether
  3. extractionagain extracted with methylene chloride
  4. washThe organic extracts are washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7fefc21f9657424996b491b80f457b88
出典データセット
uspto-grants-1979_08
特許番号
US04163852

関連ノート

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