p-Toluenesulfonic acid monohydrate → 5-methyl-2-[1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-1H-imidazol-2-yl]pyridine

HRID 52352ノート

反応式

HRID 52352 の反応式
[CH3:1][C:2]1[CH:3]=[N:4][C:5]([C:8]2[N:9]([C:18]3[CH:23]=[CH:22][C:21]([S:24]([CH3:27])(=[O:26])=[O:25])=[CH:20][CH:19]=3)[CH2:10][C:11](O)([C:13]([F:16])([F:15])[F:14])[N:12]=2)=[CH:6][CH:7]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([C:18]3[CH:23]=[CH:22][C:21]([S:24]([CH3:27])(=[O:26])=[O:25])=[CH:20][CH:19]=3)[CH:10]=[C:11]([C:13]([F:15])([F:14])[F:16])[N:12]=2)=[N:4][CH:3]=1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 199633603-methyl-6-[4-hydroxy-1-[4-(methylsulfonyl)phenyl]-4-(trifluoromethyl)-4,5-dihydro-1H-imidazol-2-yl]pyridine

生成物 1

HCID 108098545-methyl-2-[1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-1H-imidazol-2-yl]pyridine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of the 4,5-dihydro-imidazole of step 2 (10 mmol) and p-toluenesulfonic acid monohydrate (2 mmol) in toluene (200 ml) is heated to reflux for 24 hours. The reaction mixture is cooled and the solvent removed under reduced pressure. The crude mixture is chromatographed on silica gel using mixtures of ethyl acetate and acetone as eluants to give the desired product.

後処理

  1. temperatureis heated
  2. temperatureto reflux for 24 hours
  3. temperatureThe reaction mixture is cooled
  4. customthe solvent removed under reduced pressure
  5. customThe crude mixture is chromatographed on silica gel using mixtures of ethyl acetate and acetone as eluants

出典と根拠

ORDレコード
ord-51e4937b69ca4e239267b0e2768a42e7
出典データセット
uspto-grants-1997_04
特許番号
US05616601

反応ノート

読み込み中…