Diethyl Malonate → Diethyl 2,4,5-trimethoxybenzylidenemalonate

HRID 354684

反応式

HRID 354684 の反応式
[CH3:1][O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([O:13][CH3:14])=[CH:7][C:4]=1[CH:5]=O.[C:15]([O:23][CH2:24][CH3:25])(=[O:22])[CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18].N1CCCCC1>C1(C)C=CC=CC=1.C(O)(=O)C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([O:13][CH3:14])=[CH:7][C:4]=1[CH:5]=[C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:15]([O:23][CH2:24][CH3:25])=[O:22]

参加物

6

反応物 3

HCID 7761Diethyl MalonateHCID 8082PiperidineHCID 205252,4,5-Trimethoxybenzaldehyde

生成物 1

HCID 13103748Diethyl 2,4,5-trimethoxybenzylidenemalonate収率 87.8%

試薬・触媒・溶媒 2

HCID 243Benzoic Acid触媒HCID 1140Toluene溶媒

実験手順

In 80 ml of toluene is dissolved 5.9 g of 2,4,5-trimethoxybenzaldehyde, followed by addition of 4.8 g of diethyl malonate, 0.3 ml of piperidine and 0.3 g of benzoic acid. The mixture is heated under reflux for 4 hours, water being removed via an ester tube. After cooling, the solvent is distilled off under reduced pressure and the residual crystals are recovered by filtration with n-hexane to give 8.9 g (87.3%) of diethyl 2,4,5-trimethoxybenzylidenemalonate, m.p. 86°-87° C.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 4 hours
  3. customwater being removed via an ester tube
  4. temperatureAfter cooling
  5. distillationthe solvent is distilled off under reduced pressure
  6. filtrationthe residual crystals are recovered by filtration with n-hexane

出典と根拠

ORDレコード
ord-6f93c1aa4d9b48f088f2bd32e5d97be1
出典データセット
uspto-grants-1983_03
特許番号
US04376777

関連ノート

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