Butanedione → HCID 178432086、化合物

HRID 1089737ノート

反応式

HRID 1089737 の反応式
[NH2:1][C:2]1[C:11]([NH2:12])=[CH:10][CH:9]=[C:8]2[C:3]=1[N:4]=[C:5]([OH:14])[C:6]([OH:13])=[N:7]2.[CH3:15][C:16](=O)[C:17](=O)[CH3:18]>O>[OH:14][C:5]1[C:6]([OH:13])=[N:7][C:8]2[C:3]([N:4]=1)=[C:2]1[C:11](=[CH:10][CH:9]=2)[N:12]=[C:17]([CH3:18])[C:16]([CH3:15])=[N:1]1

参加物

4

反応物 2

HCID 650ButanedioneHCID 178507339HCID 178507339、化合物

生成物 1

HCID 178432086HCID 178432086、化合物収率 64%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
25 °C

実験手順

A mixture of 0,5 g (2,6 mmol) 5,6-diamino-2,3-dihydroxyquinoxaline and 10 ml water was at 50° C. added a solution of 0,45 g (5,2 mmol) 2,3-butanedione in 5 ml water. The reaction mixture was stirred at 50° for 4 h. After cooling to 25° C., the precipitate was filtered off and washed with water. The crude product was dissolved in 2N sodium hydroxide and reprecipitated with 2N hydrochloric acid to pH 6-7 to give 0,4 g (64%) 2,3-dihydroxy-8,9-dimethylpyrazino(2,3-f)quinoxaline, m.p.>300° C. NMR (DMSO-d : 7.27 (lH,d), 6,93 (lH,d), 2.07 (6H,s).

後処理

  1. customwas at 50° C.
  2. filtrationthe precipitate was filtered off
  3. washwashed with water
  4. dissolutionThe crude product was dissolved in 2N sodium hydroxide
  5. customreprecipitated with 2N hydrochloric acid to pH 6-7

出典と根拠

ORDレコード
ord-25e563a0501c49d797126d15bd545007
出典データセット
uspto-grants-1992_01
特許番号
US05079250

反応ノート

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