Potassium Permanganate → HCID 17977726、化合物

HRID 274433ノート

反応式

HRID 274433 の反応式
[CH2:1]([O:8][C:9]1[C:14]([O:15][CH3:16])=[CH:13][C:12]([CH:17]([C:19]2[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=2)[OH:18])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Mn]([O-])(=O)(=O)=O.[K+]>O>[N:21]1[CH:22]=[CH:23][CH:24]=[C:19]([C:17]([C:12]2[CH:11]=[CH:10][C:9]([O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[C:14]([O:15][CH3:16])[CH:13]=2)=[O:18])[CH:20]=1

参加物

4

反応物 2

HCID 516875Potassium Permanganate2 回HCID 13365804alpha-[4-(Benzyloxy)-3-methoxyphenyl]-3-pyridinemethanol

生成物 1

HCID 17977726HCID 17977726、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

ba) 3.2 g of alpha-[4-(benzyloxy)-5-methoxyphenyl]-3-pyridinemethanol suspended in 50 ml of water are treated with 2.5 g of potassium permanganate, whereupon the mixture is stirred at 90° for 30 minutes After adding a further 1.0 g of potassium permanganate and stirring for a further 30 minutes at 90° the mixture is cooled to room temperature and extracted twice with 150 ml of ethyl acetate each time. The combined ethyl acetate phases are washed with sodium chloride solution, dried over sodium sulfate and evaporated. The thus-obtained residue is chromatographed on 50 g of silica gel with ethyl acetate. After recrystallization from methylene chloride/hexane there is obtained 4-(benzyloxy)-3-methoxyphenyl 3-pyridyl ketone of m.p. 76°.

後処理

  1. stirringstirring for a further 30 minutes at 90° the mixture
  2. extractionextracted twice with 150 ml of ethyl acetate each time
  3. washThe combined ethyl acetate phases are washed with sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customThe thus-obtained residue is chromatographed on 50 g of silica gel with ethyl acetate
  7. customAfter recrystallization from methylene chloride/hexane there

出典と根拠

ORDレコード
ord-8cbba5fcbe45472ea4509943df71f92a
出典データセット
uspto-grants-1995_02
特許番号
US05389653

反応ノート

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