聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 4-Chloro-1-(2-chloro-4-iodobenzyl)-2-methylimidazole-5-carbaldehyde

HRID 1828811笔记

反应方程式

HRID 1828811 反应方程式
[Cl:1][C:2]1[NH:6][C:5]([CH3:7])=[N:4][C:3]=1[CH:8]=[O:9].C(=O)([O-])[O-].[K+].[K+].[Cl:16][C:17]1[CH:24]=[C:23]([I:25])[CH:22]=[CH:21][C:18]=1[CH2:19]Br.O>CN(C)C=O.[Cl-].[Na+].O>[Cl:1][C:2]1[N:6]=[C:5]([CH3:7])[N:4]([CH2:19][C:18]2[CH:21]=[CH:22][C:23]([I:25])=[CH:24][C:17]=2[Cl:16])[C:3]=1[CH:8]=[O:9]

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 11430碳酸钾HCID 20061014HCID 20061014，化合物HCID 220586831-(溴甲基)-2-氯-4-碘苯

产物 1

HCID 155242134-Chloro-1-(2-chloro-4-iodobenzyl)-2-methylimidazole-5-carbaldehyde

试剂、催化剂与溶剂 2

HCID 6228N,N-二甲基甲酰胺溶剂HCID 57417360Sodium chloride; water溶剂

实验过程

To a solution of 5-chloro-2-methylimidazole-4-carbaldehyde (433 mg) in N,N-dimethylformamide (4.3 ml) were added potassium carbonate powder (616 mg) and 2-chloro-4-iodobenzyl bromide (1.2 equivalents) under ice-cooling and the mixture was stirred at room temperature for 2.5 hr. To the reaction mixture were added water and saturated brine, and the resulting product was extracted twice with ethyl acetate. The organic layers were combined, washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1) to give 4-chloro-1-(2-chloro-4-iodobenzyl)-2-methylimidazole-5-carbaldehyde (1.01 g) as a white powder.

后处理

  1. temperaturecooling
  2. extractionthe resulting product was extracted twice with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1)

来源与证据

ORD记录
ord-d1c549416f19477283c7bc6406b9439c
来源数据集
uspto-grants-2006_06
专利号
US07060721B1

反应笔记

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