Ethanol → 5-Isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-3-methoxyethoxycarbonyl-4-(3-ethynylphenyl)pyridine

HRID 467123

반응식

HRID 467123 반응식
[C:1]([C:3]1[CH:4]=C([CH:8]=[CH:9][CH:10]=1)C=O)#[CH:2].[NH2:11]/[C:12](/[CH3:20])=[CH:13]\[C:14]([O:16][CH:17]([CH3:19])[CH3:18])=[O:15].[C:21]([O:27][CH2:28][CH2:29][O:30][CH3:31])(=[O:26])[CH2:22][C:23]([CH3:25])=O.[CH2:32](O)[CH3:33]>>[CH:17]([O:16][C:14]([C:13]1[CH:23]([C:25]2[CH:8]=[CH:9][CH:10]=[C:3]([C:1]#[CH:2])[CH:4]=2)[C:22]([C:21]([O:27][CH2:28][CH2:29][O:30][CH3:31])=[O:26])=[C:32]([CH3:33])[NH:11][C:12]=1[CH3:20])=[O:15])([CH3:19])[CH3:18]

참가 물질

5

반응물 4

HCID 702EthanolHCID 897342-Methoxyethyl acetoacetateHCID 27716443-EthynylbenzaldehydeHCID 111372742-Butenoic acid, 3-amino-, 1-methylethyl ester

생성물 1

HCID 198134195-Isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-3-methoxyethoxycarbonyl-4-(3-ethynylphenyl)pyridine수율 53%

실험 절차

In 30 ml of dry ethyl alcohol was dissolved 1.3 g (10 mmol) of 3-ethynylbenzaldehyde, and 1.43 g (10 mmol) of isopropyl 3-aminocrotonate and 1.6 g (10 mmol) of methoxyethyl acetoacetate were successively added thereto at room temperature. The admixture was reacted under reflux with heating for 12 hours. After completing the reaction, the reaction solution was distilled away under reduced pressure and purified by subjecting to silica gel column chromatography [eluent: n-hexane-chloroform (1 : 1) to chloroform]to give 2.1 g of the chloroform (1 : 1) to chloroform] to give 2.1 g of the desired compound (yield: 53%).

후처리

  1. additionwere successively added
  2. customat room temperature
  3. customThe admixture was reacted
  4. temperatureunder reflux
  5. temperaturewith heating for 12 hours
  6. customthe reaction
  7. distillationthe reaction solution was distilled away under reduced pressure
  8. custompurified
  9. customto give 2.1 g of the chloroform (1 : 1) to chloroform]

출처 및 근거

ORD 기록
ord-d5704b7d097b4eca9c81603ae798a68b
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05158963

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