Phosphorus oxychloride → 3-Chloro-2-phenyl-9-(3-pyridinyl)[1,2,4]triazolo[4',3':1,6]pyrido-[2,3-b]pyrazine

HRID 221988노트

반응식

HRID 221988 반응식
O[C:2]1[N:3]=[C:4]2[CH:17]=[CH:16][C:15]([NH:18][NH:19][C:20](=O)[C:21]3[CH:26]=[CH:25][CH:24]=[N:23][CH:22]=3)=[N:14][C:5]2=[N:6][C:7]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O=P(Cl)(Cl)[Cl:30]>C(#N)C>[Cl:30][C:2]1[N:3]=[C:4]2[CH:17]=[CH:16][C:15]3=[N:18][N:19]=[C:20]([C:21]4[CH:22]=[N:23][CH:24]=[CH:25][CH:26]=4)[N:14]3[C:5]2=[N:6][C:7]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178523945N'-(2-hydroxy-3-phenylpyrido[2,3-b]pyrazin-6-yl)nicotinohydrazide

생성물 1

HCID 866526523-Chloro-2-phenyl-9-(3-pyridinyl)[1,2,4]triazolo[4',3':1,6]pyrido-[2,3-b]pyrazine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
100 °C

실험 절차

To a mixture of N′-(2-hydroxy-3-phenylpyrido[2,3-b]pyrazin-6-yl)nicotinohydrazide (3-4) (5.8 g, 16.2 mmol) in acetonitrile (1.3 mL) was added POCl3 (7.5 mL, 81 mmol), and stirred at 100° C. for overnight. The solvent was removed under reduced pressure, and to the residue was added CHCl3 and water. The organic layer was separated, dried (Na2SO4), filtered, and evaporated in vacuo. To the residue was added CHCl3, and the resulting solid was collected by filtration to yield 3-chloro-2-phenyl-9-(3-pyridinyl)[1,2,4]triazolo[4′,3′:1,6]pyrido[2,3-b]pyrazine (3-5) as an orange solid.

후처리

  1. customThe solvent was removed under reduced pressure
  2. additionto the residue was added CHCl3 and water
  3. customThe organic layer was separated
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. additionTo the residue was added CHCl3
  8. filtrationthe resulting solid was collected by filtration

출처 및 근거

ORD 기록
ord-a33d3a20a0fc4d15b3082d8170de1785
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207169B2

반응 노트

불러오는 중…