Diethyl Oxalate → Pyrido(2,3-b)pyrazine-2,3-diol

HRID 406249ノート

反応式

HRID 406249 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[C:9](OCC)(=[O:15])[C:10](OCC)=[O:11]>>[NH:8]1[C:10](=[O:11])[C:9](=[O:15])[NH:1][C:2]2[N:3]=[CH:4][CH:5]=[CH:6][C:7]1=2

参加物

3

反応物 2

HCID 7268Diethyl OxalateHCID 99562,3-Diaminopyridine

生成物 1

HCID 74947Pyrido(2,3-b)pyrazine-2,3-diol

反応条件

温度
120 °C

実験手順

A stirred suspension of 2,3-diaminopyridine (75 g, 687 mmol) in diethyl oxalate (291 ml, 2131 mmol) under N2 was heated to 120° C. After 1 h, the ethanol was distilled off the reaction mixture and the temperature was elevated to 160° C. for a further 2 hours. The reaction mixture was allowed to cool to RT and diluted with diethyl ether (200 ml). The resulting suspension was stirred for 1 hour and the solid was isolated by filtration and dried in a vacuum oven. The solid was suspended in ethanol (500 ml) and sonicated for 1 hour. The suspension was filtered and dried (vacuum oven overnight) to afford the title compound;

後処理

  1. distillationthe ethanol was distilled off the reaction mixture
  2. waitthe temperature was elevated to 160° C. for a further 2 hours
  3. temperatureto cool to RT
  4. additiondiluted with diethyl ether (200 ml)
  5. customthe solid was isolated by filtration
  6. customdried in a vacuum oven
  7. customsonicated for 1 hour
  8. filtrationThe suspension was filtered
  9. customdried (vacuum oven overnight)

出典と根拠

ORDレコード
ord-e7da28bf0b694f51a206c83aecb76ace
出典データセット
uspto-grants-2014_06
特許番号
US08754085B2

反応ノート

読み込み中…