10-(2-furylmethylene)-5H,10H-imidazo[l,2-a]indeno[1,2-e]pyrazin-4-one → 10-(2-furylmethyl)-5H,10H-imidazo[1,2-a]indeno[1,2-e]-pyrazin-4-one

HRID 1290752ノート

反応式

HRID 1290752 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[C:7]1[C:19]2[N:18]3[CH:20]=[CH:21][N:22]=[C:17]3[C:16](=[O:23])[NH:15][C:14]=2[C:13]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]1=2>[Pd].CN(C)C=O>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][CH:7]1[C:19]2[N:18]3[CH:20]=[CH:21][N:22]=[C:17]3[C:16](=[O:23])[NH:15][C:14]=2[C:13]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]1=2

参加物

4

反応物 1

HCID 7034377510-(2-furylmethylene)-5H,10H-imidazo[l,2-a]indeno[1,2-e]pyrazin-4-one

生成物 1

HCID 1891818010-(2-furylmethyl)-5H,10H-imidazo[1,2-a]indeno[1,2-e]-pyrazin-4-one

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 10-(2-furylmethylene)-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one, 100 ml of dimethylformamide and 0.15 g of 10% palladium on charcoal is hydrogenated by flushing with a stream of hydrogen at a temperature in the region of 20° C. for 2 hours. The catalyst is then filtered off under inert atmosphere and the solvent is evaporated off. The brown solid obtained (2 g) is purified by trituration in 50 ml of acetone, filtration and crystallization of the insoluble material obtained (1 g) in 80 ml of methanol. After filtration and drying at 80° C., 0.48 g of 10-(2-furylmethyl)-5H,10H-imidazo[1,2-a]indeno[1,2-e]-pyrazin-4-one is obtained, in the form of a light brown solid melting above 260° C. (Analysis % calculated C: 71.28, H: 4.32, N: 13.85, O: 10.55, % found C: 71.5, H: 4.2, N: 14.0).

後処理

  1. customby flushing with a stream of hydrogen at a temperature in the region of 20° C. for 2 hours
  2. filtrationThe catalyst is then filtered off under inert atmosphere
  3. customthe solvent is evaporated off
  4. customThe brown solid obtained (2 g)
  5. customis purified by trituration in 50 ml of acetone
  6. filtrationfiltration and crystallization of the insoluble material
  7. customobtained (1 g) in 80 ml of methanol
  8. filtrationAfter filtration
  9. customdrying at 80° C.

出典と根拠

ORDレコード
ord-f2f51ab2a852421ca98e92d0322e52f5
出典データセット
uspto-grants-1998_05
特許番号
US05753657

反応ノート

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