Triethylamine → HCID 53717583、化合物

HRID 443580ノート

反応式

HRID 443580 の反応式
[C:1]([C:4]1[NH:5][CH:6]=[NH+:7][C:8]=1[O-:9])(=[O:3])[NH2:2].C(N(CC)CC)C.[Cl:17][C:18]1[CH:26]=[CH:25][C:21]([C:22](Cl)=[O:23])=[CH:20][CH:19]=1>CN(C)C=O>[Cl:17][C:18]1[CH:26]=[CH:25][C:21]([C:22]([O:9][C:8]2[N:7]=[CH:6][NH:5][C:4]=2[C:1](=[O:3])[NH2:2])=[O:23])=[CH:20][CH:19]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 85014-Chlorobenzoyl chlorideHCID 178513830HCID 178513830、化合物

生成物 1

HCID 53717583HCID 53717583、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a suspension of 508 mg of 4-carbamoylimidazolium-5-olate and 486 mg of triethylamine in 6 ml of anhydrous dimethylformamide was added 770 mg of p-chlorobenzoyl chloride in 3 ml of anhydrous dimethylformamide at a temperature below 5° C. The mixture was stirred under ice cooling for 4 hours. The insoluble crystals were filtered off, then the filtrate were concentrated to a residue under reduced pressure, and the resulting residue was dissolved in chloroform. The chloroform solution was washed with water, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to give 5-carbamoyl-1H-imidazol-4-yl p-chlorobenzoate. The crude solid was washed with ethyl acetate to give 340 mg of pure product, m.p. 220° C. (charred).

後処理

  1. filtrationThe insoluble crystals were filtered off
  2. concentrationthe filtrate were concentrated to a residue under reduced pressure
  3. dissolutionthe resulting residue was dissolved in chloroform
  4. washThe chloroform solution was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-f7b7d1bc559f41539eaa31f8fb2d1b00
出典データセット
uspto-grants-1981_04
特許番号
US04260774

反応ノート

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