تفاعل #3488

معادلة التفاعل

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

المردود 62.5%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةat reflux for 20 min
3. 3
   أخرى13 separated as a white powder
4. 4
   ترشيحThis 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
   درجة الحرارةOn cooling
8. 8
   أخرىoff-white flakes separated
9. 9
   ترشيحFiltration
10. 10
    أخرىdrying

الإجراء التجريبي

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.

المصدر