تفاعل #169202
ord-e3eb65687a5b40aca63272abc8d1d7f7
معادلة التفاعل
3-aminopyrazole
diethyl oxalacetate sodium salt
acetic acid
→
title compound
المردود 28.4%
6-Hydroxy-1H-pyrazolo[3,4-b]pyridine-4-carboxylic acid ethyl ester
المردود 28.4%
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
85°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةthen cooled to room temperature
- 2ترشيحfiltered
- 3غسيلThe precipitate was washed with water
- 4أخرىdried
الإجراء التجريبي
To a solution of 3-aminopyrazole (224 g, 2.7 mol) in water (1 L) were added a solution of diethyl oxalacetate sodium salt (567 g, 2.7 mol) in water (1.3 L) and then acetic acid in 4 portions (0.8 L). The reaction mixture was heated at 85° C. for 15 hours then cooled to room temperature and filtered. The precipitate was washed with water and then dried to afford the title compound as an orange solid (159 g, 28%). 1H NMR (250 MHz, DMSO): δ 1.35 (t, 3H), 4.36 (q, 2H), 6.69 (s, 1H), 8.16 (s, 1H).