反応 #3488

反応方程式

hydrochloride

2-chloro-4,6-diamino-1,3,5-triazine

HCl

3,5-diacetylaniline

→

2-(3,5-diacetylphenyl)amino-4,6-diamino-1,3,5-triazine

収率 62.5%

溶媒

water

反応条件

後処理

1. 1
   温度heated
2. 2
   温度at reflux for 20 min
3. 3
   その他13 separated as a white powder
4. 4
   ろ過This was filtered out
5. 5
   workup.DISSOLUTIONdissolved in 60 mL of boiling aqueous 75% methanol
6. 6
   workup.ADDITIONtreated with triethylamine (1.5 mL)
7. 7
   温度On cooling
8. 8
   その他off-white flakes separated
9. 9
   ろ過Filtration
10. 10
    その他drying

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.

出典