Phosphorus oxychloride → 4-chloro-1-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidine

HRID 1093185ノート

反応式

HRID 1093185 の反応式
[CH:1]([N:4]1[C:8]2=[N:9][C:10]([C:14]3[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=3)=[N:11][C:12](O)=[C:7]2[CH:6]=[N:5]1)([CH3:3])[CH3:2].P(Cl)(Cl)([Cl:25])=O>>[Cl:25][C:12]1[N:11]=[C:10]([C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)[N:9]=[C:8]2[N:4]([CH:1]([CH3:3])[CH3:2])[N:5]=[CH:6][C:7]=12

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 1784566311-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol

生成物 1

HCID 866293704-chloro-1-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidine収率 100%

実験手順

A suspension of 1-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol (0.76 g, 2.5 mmol) in phosphorus oxychloride (20 mL) was heated a sealed tube with a heat gun until all of the starting material was dissolved. After allowing the mixture to cool to room temperature it was concentrated to dryness under reduced pressure, leaving a pale yellow solid which was then triturated with water and collected by Buchner filtration. The solid was further washed with water and dried under house vacuum to provide 4-chloro-1-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidine (0.90 g, >100%) as a pale yellow solid. MS (ES+): 317.7, 319.8 (M+H)+

後処理

  1. temperaturewas heated a sealed tube with a heat gun until all of the starting material
  2. dissolutionwas dissolved
  3. concentrationwas concentrated to dryness under reduced pressure
  4. customleaving a pale yellow solid which
  5. customwas then triturated with water
  6. filtrationcollected by Buchner filtration
  7. washThe solid was further washed with water
  8. customdried under house vacuum

出典と根拠

ORDレコード
ord-104a55c1190f4354ac2c773e2f52e3bf
出典データセット
uspto-grants-2012_03
特許番号
US08129371B2

反応ノート

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