4-Hydrazinylimidazo[1,2-a]quinoxaline → HCID 10797569, 화합물

HRID 1954701노트

반응식

HRID 1954701 반응식
[NH:1]([C:3]1[C:4]2[N:5]([CH:13]=[CH:14][N:15]=2)[C:6]2[C:11]([N:12]=1)=[CH:10][CH:9]=[CH:8][CH:7]=2)N>[Ni].O>[CH:13]1[N:5]2[C:6]3[C:11]([N:12]=[C:3]([NH2:1])[C:4]2=[N:15][CH:14]=1)=[CH:10][CH:9]=[CH:8][CH:7]=3

참가 물질

4

반응물 1

HCID 232937004-Hydrazinylimidazo[1,2-a]quinoxaline

생성물 1

HCID 10797569HCID 10797569, 화합물수율 108.2%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 962Water용매

실험 절차

A mixture of 0.17 g of 4-hydrazinoimidazo[1,2-a]quinoxaline and 3.4 ml of Raney nickel in 20 ml of water is refluxed for 1.5 h. After cooling down, the mixture is filtered on Celite, followed by washing with methanolic chloroform. The filtrate is concentrated under vacuum and extracted with ethyl acetate. The organic extracts are then washed with saturated NaCl, dried and evaporated, thereby obtaining 0.17 g of imidazo[1,2-a]quinoxalin-4-amine. M.p. (DSC)=205.3° C. (onset); IR (KBr): 3301, 3143, 1653, 1525 cm-1 ; 1 -NMR (CDCl3): δ8.0 (1H,s), 7.8÷7.45 (3H,m), 7.45÷7.2 (2H,m), 5.8 (2H,sb); UV (EtOH): λmax =229, 295, 331 nm. Elementary analysis for C10H3N4 (m.w. 184.20): calcd. C 65.21, H 4.38, N 30.42%; found C 65.48, H 4.71, N 30.10%;.

후처리

  1. temperatureis refluxed for 1.5 h
  2. temperatureAfter cooling down
  3. filtrationthe mixture is filtered on Celite
  4. washby washing with methanolic chloroform
  5. concentrationThe filtrate is concentrated under vacuum
  6. extractionextracted with ethyl acetate
  7. washThe organic extracts are then washed with saturated NaCl
  8. customdried
  9. customevaporated

출처 및 근거

ORD 기록
ord-a656ff87048840a485c8aabb5ac14c05
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06124287

반응 노트

불러오는 중…