Hydrochloric Acid → 2-(3,5-Diacetylphenyl)amino-4,6-diamino-1,3,5-triazine

HRID 3392

反応式

HRID 3392 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([CH:8]=[C:9]([C:11](=[O:13])[CH3:12])[CH:10]=1)[NH2:7])(=[O:3])[CH3:2].Cl[C:15]1[N:20]=[C:19]([NH2:21])[N:18]=[C:17]([NH2:22])[N:16]=1.Cl>O>[C:1]([C:4]1[CH:5]=[C:6]([NH:7][C:15]2[N:20]=[C:19]([NH2:21])[N:18]=[C:17]([NH2:22])[N:16]=2)[CH:8]=[C:9]([C:11](=[O:13])[CH3:12])[CH:10]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 188311,3,5-Triazine-2,4-diamine, 6-chloro-HCID 463010Cni H1894

生成物 1

HCID 4843242-(3,5-Diacetylphenyl)amino-4,6-diamino-1,3,5-triazine収率 62.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Compound No. 13: A suspension of 3,5-diacetylaniline (1.95 g) in water (10 mL) was treated with 2-chloro-4,6-diamino-1,3,5-triazine (1.455 g) and concentrated HCl (0.1 mL) and heated at reflux for 20 min. After cooling the hydrochloride of Compound No. 13 separated as a white powder. This was filtered out, dissolved in 60 mL of boiling aqueous 75% methanol and treated with triethylamine (1.5 mL). On cooling, off-white flakes separated. Filtration and drying gave 1.79 g of 2-(3,5-diacetylphenyl)amino-4,6-diamino-1,3,5-triazine, mp 271°-2° C.

後処理

  1. temperatureheated
  2. temperatureat reflux for 20 min
  3. custom13 separated as a white powder
  4. filtrationThis was filtered out
  5. dissolutiondissolved in 60 mL of boiling aqueous 75% methanol
  6. additiontreated with triethylamine (1.5 mL)
  7. temperatureOn cooling
  8. customoff-white flakes separated
  9. filtrationFiltration
  10. customdrying

出典と根拠

ORDレコード
ord-f5ab73fd88e543f2b4cd602c407b93f7
出典データセット
uspto-grants-1998_03
特許番号
US05733932

関連ノート

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