1,1'-Carbonyldiimidazole → HCID 178493957、化合物

HRID 1973362ノート

反応式

HRID 1973362 の反応式
[CH3:1][O:2][C:3]1[C:4]([C:13]([OH:15])=O)=[N:5][C:6]2[C:11]([N:12]=1)=[CH:10][CH:9]=[CH:8][CH:7]=2.C1N=CN(C(N2C=NC=C2)=O)C=1.[NH2:28][C:29]1[NH:33][N:32]=[N:31][N:30]=1>O1CCCC1.CN(C)C=O>[CH3:1][O:2][C:3]1[C:4]([C:13]([NH:28][C:29]2[NH:33][N:32]=[N:31][N:30]=2)=[O:15])=[N:5][C:6]2[C:11]([N:12]=1)=[CH:10][CH:9]=[CH:8][CH:7]=2

参加物

6

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 214913233-Methoxyquinoxaline-2-carboxylic acidHCID 178509299HCID 178509299、化合物

生成物 1

HCID 178493957HCID 178493957、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

3Methoxy-2-quinoxalinecarboxylic acid (1.5 g) and N,N-carbonyldiimidazole (1.2 g) in tetrahydrofuran (50 ml) were heated under reflux for 15 minutes. 5-Amino-1H-tetrazole (0.7 g) in dimethylformamide (5 ml) was added and the solution was heated under reflux for 1 hour. The crystalline solid was collected and stirred with dilute hydrochloric acid (25 ml., 2N) and the solid was filtered off and dried. It had m.p. 260° (d) (45%).

後処理

  1. temperatureunder reflux for 15 minutes
  2. temperaturethe solution was heated
  3. temperatureunder reflux for 1 hour
  4. customThe crystalline solid was collected
  5. filtrationthe solid was filtered off
  6. customdried

出典と根拠

ORDレコード
ord-f54e645f40f74558a9bcb0a4db3f3289
出典データセット
uspto-grants-1976_12
特許番号
US03997535

反応ノート

読み込み中…