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

HRID 1836992노트

반응식

HRID 1836992 반응식
[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[C:7]([N:9](C)[C:10]1[N:15]=[C:14]([C:16]2[CH:21]=[CH:20][C:19]([S:22]([CH3:25])(=[O:24])=[O:23])=[CH:18][CH:17]=2)[CH:13]=[C:12]([C:26]([F:29])([F:28])[F:27])[N:11]=1)=O>C(O)C.Cl>[NH3:4].[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[CH2:7][NH:9][C:10]1[N:15]=[C:14]([C:16]2[CH:17]=[CH:18][C:19]([S:22]([CH3:25])(=[O:24])=[O:23])=[CH:20][CH:21]=2)[CH:13]=[C:12]([C:26]([F:29])([F:27])[F:28])[N:11]=1

참가 물질

5

반응물 1

HCID 69565578(5-methyl-1H-imidazol-4-yl)methyl[4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidin-2yl]formamide

생성물 2

HCID 222AmmoniaHCID 23497469N-[(5-methyl-1H-imidazol-4-yl)methyl]-4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidine-2-amine수율 110.7%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

A solution of crude (5-methyl-1H-imidazol-4-yl)methyl[4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidin-2yl]formamide (0.27 g, 0.615 mmol) in ethanol (10 ml) and 2N hydrochloric acid (10 ml) was heated under reflux for 2 h. The solvents were then evaporated and the residue basified with 0.880 ammonia and extracted with DCM. The dried organic phase was evaporated onto silica gel and this mixture was purified on a silica gel SPE cartridge. Elution with DCM:ethanol:0.880 ammonia, 91:8:1, gave the title compound as a colourless crystalline solid (0.14 g).

후처리

  1. temperatureunder reflux for 2 h
  2. customThe solvents were then evaporated
  3. extractionextracted with DCM
  4. customThe dried organic phase was evaporated onto silica gel
  5. customthis mixture was purified on a silica gel SPE cartridge
  6. washElution with DCM

출처 및 근거

ORD 기록
ord-b954b3eeb37b487f8762052bfafbac6a
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06780870B2

반응 노트

불러오는 중…