4-Cyanophenol → Isopropyl alcohol isopropyl ether

HRID 261070

반응식

HRID 261070 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 21202047Isopropyl alcohol isopropyl ether수율 23%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
80 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-7fefc21f9657424996b491b80f457b88
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04163852

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