Diethyl Malonate → HCID 18784169, 화합물

HRID 1108753노트

반응식

HRID 1108753 반응식
[C:1]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:2][C:3]([O:5]CC)=O.CC(C)([O-])C.[K+].[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH:28]=[CH:29][C:30](=[O:32])[CH3:31])[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]>C(O)C>[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH:28]2[CH2:29][C:30](=[O:32])[CH2:31][C:3](=[O:5])[CH:2]2[C:1]([O:9][CH2:10][CH3:11])=[O:8])[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]

참가 물질

5

반응물 3

HCID 7761Diethyl MalonateHCID 847484-(3,4-Dimethoxyphenyl)but-3-en-2-oneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 18784169HCID 18784169, 화합물수율 871.4%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

Diethyl malonate (73. 7 g) was dissolved in ethanol (700 ml), and then potassium tert-butoxide (51.6 g) was gradually added thereto. A solution of 4-(3,4-dimethoxyphenyl)-3-buten-2-one (79.1 g) in ethanol (500 ml) was added dropwise, and the mixture was refluxed for 1.5 hours. After distilling off the reaction solvent under reduced pressure, ice water was poured over it and it was adjusted to pH4 with concentrated hydrochloric acid. The deposited crystals were filtered by suction, washed with water and then air-dried to give 122 g of ethyl 2-(3,4-dimethoxyphenyl)-4,6-dioxocyclohexane carboxylate (99.6%).

후처리

  1. temperaturethe mixture was refluxed for 1.5 hours
  2. distillationAfter distilling off the reaction solvent under reduced pressure, ice water
  3. additionwas poured over it and it
  4. filtrationThe deposited crystals were filtered by suction
  5. washwashed with water
  6. customair-dried

출처 및 근거

ORD 기록
ord-9c21202cffce45829b9f67d9e3bde488
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06069176

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