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

HRID 467123

反応式

HRID 467123 の反応式
[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]

参加物

5

反応物 4

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

生成物 1

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

実験手順

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%).

後処理

  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]

出典と根拠

ORDレコード
ord-d5704b7d097b4eca9c81603ae798a68b
出典データセット
uspto-grants-1992_10
特許番号
US05158963

関連ノート

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