聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 1-(4-Pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene

HRID 324035

反应方程式

HRID 324035 反应方程式
CO[CH:3](OC)[C:4]1[C:9]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:8][C:7]([O:16][CH3:17])=[C:6]([O:18][CH3:19])[C:5]=1CO.[CH3:24][O:25][C:26](=[O:33])/[CH:27]=[CH:28]\[C:29]([O:31][CH3:32])=[O:30].[CH3:34]S(O)(=O)=O.O>C(O)(=O)C.C1(C)C=CC=CC=1>[N:13]1[CH:12]=[CH:11][C:10]([C:9]2[C:4]3[C:3](=[CH:8][C:7]([O:16][CH3:17])=[C:6]([O:18][CH3:19])[CH:5]=3)[CH:34]=[C:27]([C:26]([O:25][CH3:24])=[O:33])[C:28]=2[C:29]([O:31][CH3:32])=[O:30])=[CH:15][CH:14]=1

参与物

7

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 6395甲基磺酸HCID 5271565顺丁烯二酸二甲酯HCID 220073783,4-Dimethoxy-6-(4-pyridyl) hydroxymethylbenzaldehyde dimethylacetal

产物 1

HCID 117286421-(4-Pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene

试剂、催化剂与溶剂 2

HCID 176醋酸溶剂HCID 1140甲苯溶剂

实验过程

To a solution of 3,4-dimethoxy-6-(4-pyridyl)hydroxymethylbenzaldehyde dimethyl acetal (18.4 g) in a mixture of acetic acid (50 ml) and toluene (50 ml) is added maleic acid dimethyl ester (8.64 ml), and the mixture is refluxed for one hour. To the mixture is added methanesulfonic acid (9.33 ml), and the mixture is refluxed for 8 hours while the generated water is removed by using a Dean-stark apparatus. The mixture is cooled to room temperature and concentrated. The residue is dissolved in chloroform, and the pH value thereof is adjusted to pH 8 with an aqueous potassium carbonate solution. The mixture is extracted with chloroform, and the extract is washed, dried, concentrated, and the residue is crystallized from ether to give 1-(4-pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene (13.5 g).

后处理

  1. temperaturethe mixture is refluxed for one hour
  2. customis removed
  3. concentrationconcentrated
  4. dissolutionThe residue is dissolved in chloroform
  5. extractionThe mixture is extracted with chloroform
  6. washthe extract is washed
  7. customdried
  8. concentrationconcentrated
  9. customthe residue is crystallized from ether

来源与证据

ORD记录
ord-9155ad3721b84f87879551e41d65dcde
来源数据集
uspto-grants-2001_04
专利号
US06214996B1

关联笔记

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