Piperidine → Minoxidil

HRID 1087878

反応式

HRID 1087878 の反応式
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

参加物

4

反応物 2

HCID 8082PiperidineHCID 22164170HCID 22164170、化合物

生成物 1

HCID 4201Minoxidil収率 75%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a57ed989de0e4fd9ab68fa078da0ba4b
出典データセット
uspto-grants-1990_10
特許番号
US04960888

関連ノート

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