1,4-Dioxane hydrochloride → HCID 178498852, compound

Temperature

60 °C

Commercially available 5-hydroxypyrazine-2-carboxylic acid (1.00 g, 7.14 mmol) was dissolved in methanol (5 mL), and a 4N hydrochloric acid/dioxane solution (25 mL) was added, followed by stirring at 60° C. for 1.5 hours and heating to reflux at 80° C. for 2.5 hours. The reaction solution was brought back to room temperature, the solvent was distilled off under reduced pressure, and ethyl acetate (20 mL) was added to the resulting residue to allow it to be suspended. The resulting precipitate was filtered off, and washed with ethyl acetate, followed by vacuum drying, to afford the desired compound (673 mg, yield 61%) as an orange-brown solid.

1. temperatureheating
2. temperatureto reflux at 80° C. for 2.5 hours
3. customwas brought back to room temperature
4. distillationthe solvent was distilled off under reduced pressure, and ethyl acetate (20 mL)
5. additionwas added to the resulting residue
6. filtrationThe resulting precipitate was filtered off
7. washwashed with ethyl acetate
8. customdrying

ORD record

ord-1f3cc2728f13492ba1aa3434ca279db1

Source dataset

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08415359B2