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HRID1071459

反应详情

EQUATION

反应方程式

HRID 1071459 的结构方程式

REACTANTS

反应物

4
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：Nc1nc(N)nc(Cl)n1
HCID18831

6-Chloro-1,3,5-triazine-2,4-diamine

C3H4ClN5

结构：CC(=O)c1cc(N)cc(C(C)=O)c1
HCID463010

1,1'-(5-Amino-1,3-phenylene)di(ethan-1-one)

C10H11NO2

结构：CC(=O)c1cc(NC(=N)NC(=N)N)cc(C(C)=O)c1.Cl
HCID178418457

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)c1cc(Nc2nc(N)nc(N)n2)cc(C(C)=O)c1
HCID484324

Ethanone, 1,1'-(5-((4,6-diamino-1,3,5-triazin-2-yl)amino)-1,3-phenylene)bis-

C13H14N6O2

收率 62.5%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

PROCEDURE

实验过程

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.

WORKUP

后处理

  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