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

HRID 331194노트

반응식

HRID 331194 반응식
[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

참가 물질

4

반응물 2

HCID 971Oxalic AcidHCID 59183,4-Diaminopyridine

생성물 1

HCID 107970835-Trifluoromethyl-quinazoline-2,4-diamine수율 81.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1686f39fb6664013ac82f03e6c451286
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877757B2

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