Methanol → 2-(1H-1,2,4-triazol-3-yl)acetic acid

Temperature

100 °C

A mixture of ethyl 1H-1,2,4-triazol-3-ylacetate obtained in Reference Example 14 (900 mg, 5.80 mmol), 4N aqueous sodium hydroxide solution (7.25 mL, 29.0 mmol), water (10 mL), methanol (10 mL) and THF (10 mL) was stirred at 100° C. for 2 hr. The reaction mixture was concentrated under reduced pressure, the residue was acidified with 1N hydrochloric acid, and the mixture was concentrated under reduced pressure. Ethanol was added to the residue, and the insoluble material was filtered off, and the filtrate was concentrated. The residue was crystallized from toluene to give the title compound as a white powder (369 mg, 50%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. concentrationthe mixture was concentrated under reduced pressure
3. additionEthanol was added to the residue
4. filtrationthe insoluble material was filtered off
5. concentrationthe filtrate was concentrated
6. customThe residue was crystallized from toluene

ORD record

ord-ec4c4f925dda47fb8817c9f10dff6bc8

Source dataset

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07915267B2