4-Hydrazinylimidazo[1,2-a]quinoxaline → HCID 10797569、化合物

HRID 1954701ノート

反応式

HRID 1954701 の反応式
[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

参加物

4

反応物 1

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

生成物 1

HCID 10797569HCID 10797569、化合物収率 108.2%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 962Water溶媒

実験手順

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%;.

後処理

  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

出典と根拠

ORDレコード
ord-a656ff87048840a485c8aabb5ac14c05
出典データセット
uspto-grants-2000_09
特許番号
US06124287

反応ノート

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