Potassium Permanganate → HCID 17977726, 화합물

HRID 725298노트

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HRID 725298 반응식
[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

참가 물질

4

반응물 2

HCID 516875Potassium Permanganate2회HCID 13365804alpha-[4-(Benzyloxy)-3-methoxyphenyl]-3-pyridinemethanol

생성물 1

HCID 17977726HCID 17977726, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-e5faf829a32b4edc8026d7c7d4c44d29
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705703

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