Diethyl Malonate → Diethyl 2,4,5-trimethoxybenzylidenemalonate

HRID 354684

반응식

HRID 354684 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 13103748Diethyl 2,4,5-trimethoxybenzylidenemalonate수율 87.8%

시약·촉매·용매 2

HCID 243Benzoic Acid촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f93c1aa4d9b48f088f2bd32e5d97be1
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04376777

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