Propionic anhydride → 6-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline

HRID 1581127ノート

反応式

HRID 1581127 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([NH2:12])[C:6]([NH2:13])=[N:5]2.[C:14](OC(=O)CC)(=O)[CH2:15][CH3:16]>C(O)(=O)CC>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]1[NH:12][C:14]([CH2:15][CH3:16])=[N:13][C:6]1=[N:5]2

参加物

4

反応物 2

HCID 31263Propionic anhydrideHCID 125173906-Chloroquinoxaline-2,3-diamine

生成物 1

HCID 1784375416-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline収率 88.1%

試薬・触媒・溶媒 1

HCID 1032Propionic Acid溶媒

実験手順

78 G (0.4 mole) of 6-chloro-2,3-diamino-quinoxaline were dissolved in 500 ml of anhydrous propionic acid and 105 g (0.8 mole) of propionic anhydride were added thereto. The reaction mixture was heated to the boil under reflux for 5 hours. After cooling, the solvent was distilled off in vacuo, the residue was taken up in dilute sodium hydroxide solution, the mixture was filtered, the filtrate was acidified with dilute hydrochloric acid and the resulting precipitate was filtered off. It was well washed with water and dried in vacuo at 110°C. 82 g (representing 88% of theory) of 6-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline of melting point 190°C (decomposition) were obtained.

後処理

  1. temperatureThe reaction mixture was heated to the boil
  2. temperatureunder reflux for 5 hours
  3. temperatureAfter cooling
  4. distillationthe solvent was distilled off in vacuo
  5. filtrationthe mixture was filtered
  6. filtrationthe resulting precipitate was filtered off
  7. washIt was well washed with water
  8. customdried in vacuo at 110°C

出典と根拠

ORDレコード
ord-4bd62135f66047e2a7e1e1aa37a7afa4
出典データセット
uspto-grants-1976_01
特許番号
US03935312

反応ノート

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