Acetonitrile → HCID 14677477、化合物

HRID 477454ノート

反応式

HRID 477454 の反応式
C[N:2]([CH3:15])[CH:3]=[CH:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=1)=O.Cl.NC1[N:19]=[CH:20][NH:21][C:22]=1[C:23]([NH2:25])=[O:24].C(=O)(O)[O-].[Na+].C(#N)C>C(O)(=O)C>[CH3:14][O:13][C:10]1[CH:9]=[CH:8][C:7]([C:5]2[N:19]3[CH:20]=[N:21][C:22]([C:23]([NH2:25])=[O:24])=[C:15]3[N:2]=[CH:3][CH:4]=2)=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 661465-Aminoimidazole-4-carboxamide hydrochlorideHCID 516892Sodium BicarbonateHCID 7224023-(Dimethylamino)-1-(4-methoxyphenyl)prop-2-en-1-one

生成物 1

HCID 14677477HCID 14677477、化合物収率 40.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A stirred mixture of 15.0 g of 3-dimethylamino-4'-methoxyacrylophenone (prepared as described in Example 8) and 9.2 g of 4-amino-5-imidazolecarboxamide hydrochloride in 450 ml of glacial acetic acid was heated at reflux for 24 hours. Evaporation of the solvent in vacuo gave a solid which was treated with saturated sodium bicarbonate solution, then washed with water and filtered to give colorless crystals. This material was treated with hot acetonitrile and collected by filtration. Recrystallization from ethanol gave 6.1 g of the desired product as yellow crystals, mp 246°-249° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 24 hours
  3. customEvaporation of the solvent in vacuo
  4. customgave a solid which
  5. washwashed with water
  6. filtrationfiltered
  7. customto give colorless crystals
  8. filtrationcollected by filtration
  9. customRecrystallization from ethanol

出典と根拠

ORDレコード
ord-fd534a1d419b46c1bf89cb3dfe7bae20
出典データセット
uspto-grants-1989_12
特許番号
US04888345

反応ノート

読み込み中…