Piperidine → Minoxidil

HRID 1087878

반응식

HRID 1087878 반응식
C([O:4][N:5]1[C:10]([NH2:11])=[CH:9][C:8](OS(C2C=CC(C)=CC=2)(=O)=O)=[N:7][C:6]1=[NH:23])(=O)C.[NH:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1>C(Cl)(Cl)Cl>[NH2:11][C:10]1[N:5]([OH:4])[C:6](=[NH:23])[N:7]=[C:8]([N:24]2[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)[CH:9]=1

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 22164170HCID 22164170, 화합물

생성물 1

HCID 4201Minoxidil수율 75%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

0.3 g (0.88 mmole) of 1-acetoxy-6-amino-1,2-dihydro-2-imino-4-(4-toluenesulfonyloxy)pyrimidine is added to a solution containing 10 ml of chloroform and 2 ml of piperidine while stirring. The mixture is refluxed under stirring for 30 minutes, then evaporated under reduced pressure. To the residue, 5 ml of ethanol and 1 ml of 1N aqueous sodium hydroxide solution are added. The mixture is set aside at room temperature for one hour, then evaporated under reduced pressure. The residue is triturated with 10 ml of water, the crystals are filtered, washed with water and dried to give 0.14 g (75% yield) of the aimed compound which shows no melting point depression when mixed with the product of Example 1.

후처리

  1. temperatureThe mixture is refluxed
  2. stirringunder stirring for 30 minutes
  3. customevaporated under reduced pressure
  4. additionTo the residue, 5 ml of ethanol and 1 ml of 1N aqueous sodium hydroxide solution are added
  5. customevaporated under reduced pressure
  6. customThe residue is triturated with 10 ml of water
  7. filtrationthe crystals are filtered
  8. washwashed with water
  9. customdried

출처 및 근거

ORD 기록
ord-a57ed989de0e4fd9ab68fa078da0ba4b
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960888

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