Nicotinic Acid → 2-Amino-4-nicotinamido-6-phenyl-s-triazine

HRID 866405

反応式

HRID 866405 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]([C:7]2[N:8]=[C:9]([NH2:14])[N:10]=[C:11]([NH2:13])[N:12]=2)=[CH:5][CH:6]=1.[C:15](O)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[N:18][CH:17]=1.P(Cl)(Cl)(Cl)=O>N1C=CC=CC=1>[NH2:13][C:11]1[N:10]=[C:9]([NH:14][C:15](=[O:22])[C:16]2[CH:21]=[CH:20][CH:19]=[N:18][CH:17]=2)[N:8]=[C:7]([C:4]2[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=2)[N:12]=1

参加物

5

反応物 3

HCID 938Nicotinic AcidHCID 7064BenzoguanamineHCID 24813Phosphorus oxychloride

生成物 1

HCID 146016342-Amino-4-nicotinamido-6-phenyl-s-triazine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

5.7 g of benzoguanamine and 4.0 g of nicotinic acid are dissolved in 300 ml of pyridine, and this solution is stirred with 5.0 g of phosphoryl chloride at room temperature. After continuing agitation at 60° C for 2 hours, the pyridine is removed by evaporation to dryness under vacuum. The residue is washed with water and fractionated and recrystallized from a mixed solution of methanol and dioxane, to yield 2-amino-4-nicotinamido-6-phenyl-s-triazine [mononicotinoylbenzoguanamine], melting point, 240° - 242° C in a yield of 2.8 g, and 2,4-bis(nicotinamido)-6-phenyl-s-triazine [dinicotinoylbenzoguanamine], melting point, 131° - 133° C in a yield of 0.7 g.

後処理

  1. customat 60° C
  2. customfor 2 hours
  3. customthe pyridine is removed by evaporation to dryness under vacuum
  4. washThe residue is washed with water
  5. customrecrystallized from a mixed solution of methanol and dioxane

出典と根拠

ORDレコード
ord-910585ea4e5d484786a9fffe1f7e900f
出典データセット
uspto-grants-1978_07
特許番号
US04098892

関連ノート

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