Dimethylformamide → (5-methyl-1H-imidazol-4-yl)methyl[4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidin-2yl]formamide

HRID 1836985노트

반응식

HRID 1836985 반응식
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[C:15]([C:17]([F:20])([F:19])[F:18])[N:14]=[C:13]([NH:21][CH:22]=[O:23])[N:12]=2)=[CH:7][CH:6]=1)(=[O:4])=[O:3].[H-].[Na+].Cl.Cl[CH2:28][C:29]1[N:30]=[CH:31][NH:32][C:33]=1C.[CH3:35]N(C)C=O>>[CH3:28][C:29]1[NH:30][CH:31]=[N:32][C:33]=1[C:22]([N:21]([CH3:35])[C:13]1[N:12]=[C:11]([C:8]2[CH:9]=[CH:10][C:5]([S:2]([CH3:1])(=[O:3])=[O:4])=[CH:6][CH:7]=2)[CH:16]=[C:15]([C:17]([F:19])([F:20])[F:18])[N:14]=1)=[O:23]

참가 물질

5

실험 절차

To a stirred solution of 4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidin-2-ylformamide (0.5 g, 1.54 mmol) in dry dimethylformamide (10 ml) under N2 was added sodium hydride (60% dispersion in oil, 0.16 g). The mixture was stirred for 30 mins, 4-(chloromethyl)-5-methyl-1H-imidazole, hydrochloride (0.283 g) was added and stirring was then continued at room temp for 18 h. The mixture was then partitioned between water and ethyl acetate. The extracts were dried (Na2SO4) and evaporated. The residue was then triturated with diethyl ether giving the crude title compound as a pale yellow solid (0.27 g).

후처리

  1. stirringstirring
  2. waitwas then continued at room temp for 18 h
  3. customThe mixture was then partitioned between water and ethyl acetate
  4. dry with materialThe extracts were dried (Na2SO4)
  5. customevaporated
  6. customThe residue was then triturated with diethyl ether giving the crude title compound as a pale yellow solid (0.27 g)

출처 및 근거

ORD 기록
ord-a7b13d90e138458ca8cefda020f17ec7
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06780870B2

반응 노트

불러오는 중…