Tetrabutylammonium permanganate → HCID 19072548、化合物

HRID 1955741ノート

反応式

HRID 1955741 の反応式
[C:1]1([CH3:38])[CH:6]=[CH:5][C:4]([S:7]([NH:10][C:11](=[O:37])[CH:12]([C:18]2[CH:23]=[CH:22][C:21]([CH2:24][N:25]3[C:29]([CH:30]=[O:31])=[C:28]([Cl:32])[N:27]=[C:26]3[CH2:33][CH2:34][CH2:35][CH3:36])=[CH:20][CH:19]=2)[CH:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[Mn]([O-])(=O)(=O)=[O:40].C([N+](CCCC)(CCCC)CCCC)CCC>N1C=CC=CC=1>[C:1]1([CH3:38])[CH:2]=[CH:3][C:4]([S:7]([NH:10][C:11](=[O:37])[CH:12]([C:18]2[CH:23]=[CH:22][C:21]([CH2:24][N:25]3[C:29]([C:30]([OH:40])=[O:31])=[C:28]([Cl:32])[N:27]=[C:26]3[CH2:33][CH2:34][CH2:35][CH3:36])=[CH:20][CH:19]=2)[CH:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)(=[O:9])=[O:8])=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 11760202Tetrabutylammonium permanganateHCID 19072485N-4-Tolylsulphonyl-2-[4-(2-butyl-4-chloro-5-formyl-imidazol-1-yl-methyl)-phenyl]-2-cyclopentyl-acetamide

生成物 1

HCID 19072548HCID 19072548、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

反応条件

温度
60 °C

実験手順

250 mg (0.45 mmol) of the compound from Example III are dissolved in 2.5 ml (0.45 mmol) of pyridine and 162 mg of tetrabutylammonium permanganate, dissolved in 1.5 ml of pyridine, are added at 60° C., and the mixture is stirred at 60° C. for 2 h. The pyridine is evaporated, and the residue is taken up in water, acidified with dilute HCl and extracted with ethyl acetate. The organic phase is concentrated and the residue is chromatographed on silica gel 60 using CH2Cl2 /MeOH (10:1).

後処理

  1. additionare added at 60° C.
  2. customThe pyridine is evaporated
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic phase is concentrated
  5. customthe residue is chromatographed on silica gel 60 using CH2Cl2 /MeOH (10:1)

出典と根拠

ORDレコード
ord-f55a8a9747e94994b369373934dccc4c
出典データセット
uspto-grants-1998_07
特許番号
US05776964

反応ノート

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