Acetyl chloride → HCID 11793343, 화합물

HRID 359693노트

반응식

HRID 359693 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 11793343HCID 11793343, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-67a7d951c0a24835a8e3dba520e4eaa9
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05002945

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