Acetyl chloride → HCID 11793343、化合物

HRID 359693ノート

反応式

HRID 359693 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][C:6]1[CH:7]=[CH:8][C:9]([N:12]2[CH:16]=[CH:15][N:14]=[C:13]2[S:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[N:25]([CH3:27])[CH3:26])=[N:10][CH:11]=1.C(N(CC)CC)C>C(Cl)Cl>[C:1]([NH:5][C:6]1[CH:7]=[CH:8][C:9]([N:12]2[CH:16]=[CH:15][N:14]=[C:13]2[S:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[N:25]([CH3:27])[CH3:26])=[N:10][CH:11]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 105680931-(5-Amino-2-pyridyl)-2-(2-(dimethylamino)benzylthio)imidazole

生成物 1

HCID 11793343HCID 11793343、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.26 ml of acetyl chloride is added to a mixture of 0.98 g of 1-(5-amino-2-pyridyl)-2-[2-(dimethylamino)benzylthio]imidazole, 1 ml of triethylamine and 30 ml of methylene chloride under ice-cooling. The mixture is stirred at the same temperature for 2 hours, washed with water and a saturated aqueous sodium bicarbonate solution, dried and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; chloroform:methanol=30:1), and crystallized with isopropyl ether. The crystals are collected by filtration, whereby 0.82 g of 1-(5-acetylamino-2-pyridyl)-2-[2-(dimethylamino)benzylthio]imidazole is obtained.

後処理

  1. temperaturecooling
  2. washwashed with water
  3. dry with materiala saturated aqueous sodium bicarbonate solution, dried
  4. customevaporated
  5. customto remove the solvent
  6. customThe residue is purified by silica gel column chromatography (solvent; chloroform:methanol=30:1)
  7. customcrystallized with isopropyl ether
  8. filtrationThe crystals are collected by filtration

出典と根拠

ORDレコード
ord-67a7d951c0a24835a8e3dba520e4eaa9
出典データセット
uspto-grants-1991_03
特許番号
US05002945

反応ノート

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