Triethylamine → HCID 23003633, Verbindung

Temperatur

0 °C

To a solution of 1,3-dimethylpyrazol-5-carboxylic acid (500 mg, 3.57 mmol) in a mixture of acetone (10 mL) and water (5 mL) was added triethylamine (0.75 mL, 7.13 mmol). The mixture was cooled to 0° C. in a ice-bath. Ethylchloroformate (774 mg, 7.13 mmol) was then added and the resulting mixture was stirred for 1.5 hours at 0° C. To the mixture was added sodium azide (0.844 g, 13.0 mmol), and the mixture was stirred for another 1.5 hours. The mixture was concentrated, the residue was diluted with dichloromethane and washed with water. The organic layer was dried over MgSO4 and concentrated to give desired product (203 mg, 34%). 1HNMR (CDCl3) (δ) 6.60 (s, 1H), 4.11 (s, 3H), 2.25 (s, 3H).

1. stirringthe mixture was stirred for another 1.5 hours
2. concentrationThe mixture was concentrated
3. additionthe residue was diluted with dichloromethane
4. washwashed with water
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated

ORD-Eintrag

ord-0c121372242145d69e26687f1452137d

Quelldatensatz

uspto-grants-2003_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06608077B2