Hydrochloric Acid → 6-Nitropyrido[2,3-d]pyrimidine-2,4-diamine

HRID 619133

反応式

HRID 619133 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([NH2:9])[N:3]=1.Cl.[N+:11]([CH:14]([CH:17]=O)[CH:15]=O)([O-:13])=[O:12]>C(O)C>[NH2:1][C:2]1[N:3]=[C:4]([NH2:9])[C:5]2[CH:17]=[C:14]([N+:11]([O-:13])=[O:12])[CH:15]=[N:8][C:6]=2[N:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 138632,4,6-TriaminopyrimidineHCID 313475Nitromalonaldehyde

生成物 1

HCID 110527766-Nitropyrido[2,3-d]pyrimidine-2,4-diamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

About 1 equivalent of 2,4,6-triamino pyrimidine was suspended in about 50 ml of refluxing absolute ethanol with stirring under an atmosphere of nitrogen. Concentrated HCl was added dropwise to effect solution and as soon as solution occurred, about 1.2 equivalents of nitromalonaldehyde was added all at once. Within 10 minutes, a thick reddish voluminous precipitate started forming. TLC analysis indicated the presence of a yellow spot corresponding to that of the desired product along with staring materials. The reaction mixture was stirred at reflux for 3.5 hours, immediately diluted with 30 ml of water, cooled and neutralized with concentrated NH4OH. The precipitate was collected on a funnel and was washed repeatedly with water to remove unreacted triamino pyrimidine to yield pure 2,4-diamino-6-nitropyrido[2,3-d]pyrimidine.

後処理

  1. customa thick reddish voluminous precipitate started forming

出典と根拠

ORDレコード
ord-9ed0cc1a6bef4e5dae20a018cc73b687
出典データセット
uspto-grants-1999_09
特許番号
US05958930

関連ノート

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