Imidazole → Ethyl 4-(1H-imidazol-1-yl)benzoate

HRID 846722

反応式

HRID 846722 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.F[C:7]1[CH:17]=[CH:16][C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:9][CH:8]=1.[I-].[K+].CN(C)C(=O)C>O>[N:1]1([C:7]2[CH:17]=[CH:16][C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:9][CH:8]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

参加物

6

反応物 4

HCID 795ImidazoleHCID 4875Potassium IodideHCID 31374DimethylacetamideHCID 67976Benzoic acid, 4-fluoro-, ethyl ester

生成物 1

HCID 13423940Ethyl 4-(1H-imidazol-1-yl)benzoate収率 33.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 13.6 parts of 1H-imidazole, 16.8 parts of ethyl 4-fluorobenzoate, 0.1 parts of potassium iodide and 54 parts of N,N-dimethylacetamide was stirred and refluxed for 20 hours. The reaction mixture was cooled to room temperature and poured onto a lot of water. The product was extracted a few times with benzene. The combined extracts were washed thoroughly with water, dried, filtered and evaporated. The residue was stirred in hexane. The product was filtered off and dried, yielding 7.2 parts (33.3%) of ethyl 4-(1H-imidazol-1-yl)benzoate; mp. 100.3° C. (intermediate 18).

後処理

  1. temperaturerefluxed for 20 hours
  2. extractionThe product was extracted a few times with benzene
  3. washThe combined extracts were washed thoroughly with water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. stirringThe residue was stirred in hexane
  8. filtrationThe product was filtered off
  9. customdried

出典と根拠

ORDレコード
ord-bfa5963e0e6f4035b4e62adab24026e7
出典データセット
uspto-grants-1992_08
特許番号
US05137896

関連ノート

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