碳酸钾 → Dimethyl 1-[6-(2-chloro-4-methoxyphenoxy) hexyl]-4,5-imidazole dicarboxylate

HRID 232103

反应方程式

HRID 232103 反应方程式
[NH:1]1[C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:10]([O:12][CH3:13])=[O:11])[N:3]=[CH:2]1.[Cl:14][C:15]1[CH:34]=[C:33]([O:35][CH3:36])[CH:32]=[CH:31][C:16]=1[O:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]SC1SCC(=O)N=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:14][C:15]1[CH:34]=[C:33]([O:35][CH3:36])[CH:32]=[CH:31][C:16]=1[O:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][N:1]1[C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:10]([O:12][CH3:13])=[O:11])[N:3]=[CH:2]1

参与物

5

反应物 3

HCID 11430碳酸钾HCID 768101H-咪唑-4,5-二甲酸二甲酯HCID 189218352-{[6-(2-Chloro-4-methoxyphenoxy)hexyl]thio}-4,5-dihydrothiazol-4-one

产物 1

HCID 19378829Dimethyl 1-[6-(2-chloro-4-methoxyphenoxy) hexyl]-4,5-imidazole dicarboxylate

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

Stir for 24 hours at room temperature 3.7 gm. dimethyl 4,5-imidazole dicarboxylate, 3.7 gm. of the iodide prepared in Examples 2 and 3, 25 ml. DMF and 2.8 gm potassium carbonate. Remove the solvent, extract the residue with methylene chloride, filter, wash methylene chloride fractions with water, elute on a silica column with 100% methylene chloride then 10% methanol/methylene chloride to recover the title compound.

后处理

  1. customRemove the solvent
  2. extractionextract the residue with methylene chloride
  3. filtrationfilter
  4. washwash methylene chloride fractions with water
  5. washelute on a silica column with 100% methylene chloride
  6. custom10% methanol/methylene chloride to recover the title compound

来源与证据

ORD记录
ord-44b726412bb246759a6c6e8ff26056bc
来源数据集
uspto-grants-1989_07
专利号
US04851423

关联笔记

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