Benzyl Alcohol → HCID 54532374、化合物

HRID 256580

反応式

HRID 256580 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 54532374HCID 54532374、化合物収率 87.3%

試薬・触媒・溶媒 1

HCID 2724286Titanium(IV)ethoxide触媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32045007fac441dfb7bc1bce30e13674
出典データセット
uspto-grants-1993_11
特許番号
US05258382

関連ノート

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