Dimethylcarbamoyl Chloride → 1-Dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole

HRID 127705ノート

反応式

HRID 127705 の反応式
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]1[N:11]=[C:10]([C:12]2[CH:17]=[N:16][CH:15]=[CH:14][N:13]=2)[NH:9][N:8]=1.[H-].[Na+].[CH3:20][N:21]([CH3:25])[C:22](Cl)=[O:23]>O1CCCC1>[CH3:20][N:21]([CH3:25])[C:22]([N:8]1[C:7]([C:2]2[CH:3]=[N:4][CH:5]=[CH:6][N:1]=2)=[N:11][C:10]([C:12]2[CH:17]=[N:16][CH:15]=[CH:14][N:13]=2)=[N:9]1)=[O:23]

参加物

5

反応物 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 24758Sodium hydrideHCID 135247872-(5-pyrazin-2-yl-4H-1,2,4-triazol-3-yl)pyrazine

生成物 1

HCID 202857801-Dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 2.25 g. (0.01 mole) of 3,5-dipyrazinyl-1,2,4-triazole in 200 ml. of tetrahydrofuran is added 57% sodium hydride (0.42 g., 0.01 mole). The reaction mixture is heated at reflux for one hour, cooled, and a solution of dimethylcarbamoyl chloride (1 gram, 0.01 mole) in 10 ml. of tetrahydrofuran is added dropwise. The reaction mixture is then refluxed four hours, cooled, filtered and concentrated to a solid. After recrystallization from benzene 1-dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole is obtained.

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for one hour
  3. temperaturecooled
  4. temperatureThe reaction mixture is then refluxed four hours
  5. temperaturecooled
  6. filtrationfiltered
  7. concentrationconcentrated to a solid
  8. customAfter recrystallization from benzene 1-dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole
  9. customis obtained

出典と根拠

ORDレコード
ord-7be2847047c94ec7a029b16ccc417b3f
出典データセット
uspto-grants-1981_03
特許番号
US04256887

反応ノート

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