反応 #88424

反応方程式

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

溶媒

ethanol

methanol

1,4-dioxane

反応条件

後処理

1. 1
   濃縮was then concentrated under reduced pressure
2. 2
   その他to obtain a crude product
3. 3
   その他The 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
   その他Thereafter, the generated solid was collected
7. 7
   洗浄it was washed with ethanol (30 ml)
8. 8
   その他was then dried

実験手順

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.

出典