Oxalic Acid → 5-Trifluoromethyl-quinazoline-2,4-diamine

HRID 331194ノート

反応式

HRID 331194 の反応式
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8].[C:9](O)(=[O:13])[C:10](O)=[O:11]>Cl>[NH:8]1[C:10](=[O:11])[C:9](=[O:13])[NH:1][C:2]2[CH:3]=[N:4][CH:5]=[CH:6][C:7]1=2

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 59183,4-Diaminopyridine

生成物 1

HCID 107970835-Trifluoromethyl-quinazoline-2,4-diamine収率 81.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To a suspension of 3,4-diaminopyridine (10 g, 0.068 mol) in 4N aqueous HCl (100 ml) is added oxalic acid (10.4 g, 0.082 mol) and the reaction mixture is refluxed for 20 h. The reaction mixture is cooled down and the solid precipitated is filtered, washed with water then dried under vacuum to afford 9 g (80%) of the title compound as a solid. HPLC (max plot) 98%. LC/MS: (ES+):164.3.

後処理

  1. temperaturethe reaction mixture is refluxed for 20 h
  2. temperatureThe reaction mixture is cooled down
  3. customthe solid precipitated
  4. filtrationis filtered
  5. washwashed with water
  6. customthen dried under vacuum

出典と根拠

ORDレコード
ord-1686f39fb6664013ac82f03e6c451286
出典データセット
uspto-grants-2014_11
特許番号
US08877757B2

反応ノート

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