聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 4-碘-1-甲基-1H-吡咯-2-羧酸甲酯

HRID 1129

反应方程式

HRID 1129 反应方程式
[H-].[Na+].[I:3][C:4]1[CH:5]=[C:6]([C:9]([O:11][CH3:12])=[O:10])[NH:7][CH:8]=1.I[CH3:14].O>CN(C=O)C>[CH3:14][N:7]1[CH:8]=[C:4]([I:3])[CH:5]=[C:6]1[C:9]([O:11][CH3:12])=[O:10]

参与物

6

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 6328碘甲烷HCID 24758氢化钠HCID 116732494-碘-2-吡咯羧酸甲酯

产物 1

HCID 218262474-碘-1-甲基-1H-吡咯-2-羧酸甲酯

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂2 次

实验过程

780 mg (25.9 mmol) of sodium hydride (80% in oil) and 20 ml of DMF were introduced into a three-necked flask, a solution of 6.5 g (25.9 mmol) of methyl 4-iodo-2-pyrrolecarboxylate in 50 ml of DMF was added dropwise and the mixture was stirred until gaseous emission ceased. 2.1 ml (33.6 mmol) of iodomethane were then added and the mixture was stirred at room temperature for two hours. The reaction medium was poured into water, extracted with ethyl ether, the organic phase decanted, dried over magnesium sulfate and evaporated. The residue obtained was purified by chromatography on a silica column eluted with a mixture of dichloromethane and hexane (40/60). 4.5 g (65%) of methyl N-methyl-4-iodo-2-pyrrolecarboxylate of melting point 64°-65° C. were recovered.

后处理

  1. stirringthe mixture was stirred at room temperature for two hours
  2. extractionextracted with ethyl ether
  3. customthe organic phase decanted
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customThe residue obtained
  7. customwas purified by chromatography on a silica column
  8. washeluted with a mixture of dichloromethane and hexane (40/60)
  9. custom4.5 g (65%) of methyl N-methyl-4-iodo-2-pyrrolecarboxylate of melting point 64°-65° C. were recovered

来源与证据

ORD记录
ord-8254c501c8dc491b8f88eae119f49eae
来源数据集
uspto-grants-1998_03
专利号
US05723499

关联笔记

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