반응 #88424

반응 방정식

Ethoxycarbonyl isothiocyanate

2-aminopyridine-4-carboxylic acid methyl ester

hydroxyamine hydrochloride

diisopropylethylamine

→

title compound

methyl 2-amino-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylate

용매

ethanol

methanol

1,4-dioxane

반응 조건

후처리

1. 1
   농축was then concentrated under reduced pressure
2. 2
   기타to obtain a crude product
3. 3
   기타The obtained crude product
4. 4
   workup.STIRRINGthe reaction solution was stirred at room temperature for 67 hours, at 60° C. for 5 hours
5. 5
   workup.WAITagain, at room temperature for 20 hours
6. 6
   기타Thereafter, the generated solid was collected
7. 7
   세척it was washed with ethanol (30 ml)
8. 8
   기타was then dried

실험 절차

Ethoxycarbonyl isothiocyanate (9.0 g) was added to a 1,4-dioxane (100 ml) suspension of 2-aminopyridine-4-carboxylic acid methyl ester (10 g) at an internal temperature of 19° C. to 23° C. over 20 minutes. The obtained mixture was stirred for 90 minutes at the same temperature as described above, and was then concentrated under reduced pressure to obtain a crude product. The obtained crude product was added to a mixed suspension of methanol (70 ml) and ethanol (70 ml) containing hydroxyamine hydrochloride (22.8 g) and diisopropylethylamine (34 ml), and thereafter, the reaction solution was stirred at room temperature for 67 hours, at 60° C. for 5 hours, and again, at room temperature for 20 hours. Thereafter, the generated solid was collected, and it was washed with ethanol (30 ml) and was then dried, so as to obtain the title compound (11.3 g) in the form of a white solid.

출처