Piperidine → Minoxidil

HRID 1087877

反応式

HRID 1087877 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>>[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

3

反応物 2

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

生成物 1

HCID 4201Minoxidil収率 86%

実験手順

2.02 g (10 mmoles) of 1-acetoxy-6-amino-4-chloro-1,2-dihydro-2-iminopyrimidine are added to 8 ml of piperidine at room temperature while stirring. The mixture is stirred at room temperature for 2 hours, then piperidine is evaporated under reduced pressure. The residue is taken up in a mixture containing 20 ml of ethanol and 10 ml of 1N aqueous sodium hydroxide solution and refluxed for 30 minutes, then evaporated under reduced pressure. The residue is taken up in 20 ml of water, the crystals are filtered, washed with water and dried to give 1.74 g (86% yield) of the aimed compound which shows no melting point depression when mixed with the product of Example 1.

後処理

  1. stirringThe mixture is stirred at room temperature for 2 hours
  2. custompiperidine is evaporated under reduced pressure
  3. additioncontaining 20 ml of ethanol and 10 ml of 1N aqueous sodium hydroxide solution
  4. temperaturerefluxed for 30 minutes
  5. customevaporated under reduced pressure
  6. filtrationthe crystals are filtered
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-5ccf13c07cc847a69a459dda945813ba
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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