Benzyl Alcohol → HCID 54532374, 화합물

HRID 256580

반응식

HRID 256580 반응식
[CH2:1]([O:3][C:4](=[O:16])[CH:5]([N:11]1[CH:15]=[CH:14][CH:13]=[CH:12]1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].C(O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20]C=1>CCO.CCO.CCO.CCO.[Ti]>[CH2:9]([O:8][C:6](=[O:7])[CH:5]([N:11]1[CH:12]=[CH:13][CH:14]=[CH:15]1)[C:4]([O:3][CH2:1][C:2]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:18]=1)=[O:16])[C:10]1[CH:18]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

4

반응물 2

HCID 244Benzyl AlcoholHCID 2782128diethyl 2-(1H-pyrrol-1-yl)malonate

생성물 1

HCID 54532374HCID 54532374, 화합물수율 87.3%

시약·촉매·용매 1

HCID 2724286Titanium(IV)ethoxide촉매

반응 조건

온도
110 °C

실험 절차

To a solution of 2-(pyrrol-1-yl)malonic acid diethyl ester (75.7 g) in benzyl alcohol (200 ml) was added tetraethyl titanate (3.0 g), and the resulting mixture was stirred at 110° C. for 15 hours. After removal of the benzyl alcohol under reduced pressure, the residue was chromatographed on silica gel using n-hexane/ethyl acetate (10:1) as the eluent. Fractions containing the title compound were pooled and evaporated under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane to give the title compound (102.5 g, 87.3%) as colorless crystals, mp 48.5°-49° C.

후처리

  1. customAfter removal of the benzyl alcohol under reduced pressure
  2. customthe residue was chromatographed on silica gel
  3. additionFractions containing the title compound
  4. customevaporated under reduced pressure
  5. customThe residue was recrystallized from ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-32045007fac441dfb7bc1bce30e13674
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258382

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