Piperidine → Minoxidil

HRID 1087880

반응식

HRID 1087880 반응식
C([NH:4][C:5]1[N:10]([O:11]C(=O)C)[C:9](=[NH:15])[N:8]=[C:7](OS(C2C=CC(C)=CC=2)(=O)=O)[CH:6]=1)(=O)C.[NH:27]1[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1>>[NH2:4][C:5]1[N:10]([OH:11])[C:9](=[NH:15])[N:8]=[C:7]([N:27]2[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]2)[CH:6]=1

참가 물질

3

반응물 2

HCID 8082PiperidineHCID 140351385HCID 140351385, 화합물

생성물 1

HCID 4201Minoxidil

실험 절차

76 g (0.2 mole) of 6-acetamido-1-acetoxy-1,2-dihydro-2-imino-4-(4-toluenesulfonyloxy)pyrimidine are added to 760 ml of anhydrous piperidine at a temperature of 0° to 5° C. while stirring. The mixture is stirred at the same temperature for additional 2 hours, then let to warm to room temperature and stirred for additional 24 hours. The piperidine is distilled off under reduced pressure, 500 ml of water are added to the residue, then the mixture is left to stand in the refrigerator overnight. The precipitate is filtered, washed with water and filtered by strong suction. The filter cake is washed by suspending it 3 times with 50 ml of ether each and dried to give the aimed product in a yield of 23.0 g (55%).

후처리

  1. stirringThe mixture is stirred at the same temperature for additional 2 hours
  2. stirringstirred for additional 24 hours
  3. distillationThe piperidine is distilled off under reduced pressure, 500 ml of water
  4. additionare added to the residue
  5. waitthe mixture is left
  6. customto stand in the refrigerator overnight
  7. filtrationThe precipitate is filtered
  8. washwashed with water
  9. filtrationfiltered by strong suction
  10. washThe filter cake is washed
  11. customdried

출처 및 근거

ORD 기록
ord-313df61b22ac4753b6292a101d7f2da2
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960888

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