Piperidine → Minoxidil

HRID 1087876

反応式

HRID 1087876 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 4201Minoxidil

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8a67e9b6af534d27bbc65652335ee57c
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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