(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 1836992ノート

反応式

HRID 1836992 の反応式
[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

参加物

5

反応物 1

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

生成物 2

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b954b3eeb37b487f8762052bfafbac6a
出典データセット
uspto-grants-2004_08
特許番号
US06780870B2

反応ノート

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