Piperidine → Minoxidil

HRID 1087876

반응식

HRID 1087876 반응식
C([O:4][N:5]1[C:10]([NH2:11])=[CH:9][C:8](Cl)=[N:7][C:6]1=[NH:13])(=O)C.[NH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.[OH-].[Na+]>C(O)C>[NH2:11][C:10]1[N:5]([OH:4])[C:6](=[NH:13])[N:7]=[C:8]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:9]=1

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 14798Sodium HydroxideHCID 221641673-(Acetyloxy)-6-chloro-2-imino-2,3-dihydropyrimidin-4-amine

생성물 1

HCID 4201Minoxidil

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.01 g (5 mmoles) of 1-acetoxy-6-amino-4-chloro-1,2-dihydro-2-iminopyrimidine are added under stirring to a mixture containing 10 ml of ethanol and 3 ml of piperidine. The mixture is refluxed while stirring for 30 minutes, then 5 ml of 1N aqueous sodium hydroxide solution are added and the boiling is continued for additional 30 minutes. Thereafter, the mixture is evaporated under reduced pressure and the residue is mixed with 10 ml of water. The crystalline precipitate is filtered, washed with water and dried to give the aimed compound in a yield of 0.85 g (82%), m.p.: 262°-266° C.

후처리

  1. temperatureThe mixture is refluxed
  2. stirringwhile stirring for 30 minutes
  3. customThereafter, the mixture is evaporated under reduced pressure
  4. additionthe residue is mixed with 10 ml of water
  5. filtrationThe crystalline precipitate is filtered
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-8a67e9b6af534d27bbc65652335ee57c
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960888

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