Reaktion #327980
ord-8e15ba4e94764231a73f3a5ba168eef4
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Extraktionthe aqueous phase was extracted with ethyl acetate (3×150 mL)
- 2WaschenThe combined organic phases were washed sequentially with aqueous sodium bicarbonate, 10% hydrochloric acid, water and brine
- 3TrocknenAfter drying over magnesium sulfate
- 4Filtrationfiltering
- 5Einengenconcentrating in vacuo
Vorschrift
1H-Indazole-3-carboxylic acid (5.0 g, 30.8 mmol) and carbonyl diimidazole (5.0 g, 33.9 mmol) were dissolved in N,N-dimethylformamide (150 mL) and heated to 60° C. After 2 hours, dimethylamine hydrochloride (4.0 g, 33.9) was added, and the reaction was stirred for an additional hour at 60° C. The reaction was poured into water, and the aqueous phase was extracted with ethyl acetate (3×150 mL). The combined organic phases were washed sequentially with aqueous sodium bicarbonate, 10% hydrochloric acid, water and brine. After drying over magnesium sulfate, filtering and concentrating in vacuo, the title compound was obtained.