[1,2,4]Triazolo[1,5-a]pyrazine → 5H,6H,7H,8H-(1,2,4)triazolo(1,5-a)pyrazine

Platinum(IV) oxide (2.75 g, 12.1 mmole) was added to a suspension, saturated with nitrogen, of CaO (9.30 g, 166 mmole) and [1,2,4]-triazolo[1,5-a]pyrazine (18.1 g, 151 mmole) in methoxyethanol (150 ml). The reaction mixture was stirred for 21.5 hours under a hydrogen atmosphere. The catalyst was filtered off through filter earth and washed with DCM/ethanol (9:1). The filtrate was concentrated, and the solvent was removed firstly with toluene and then with 2-propanol. The residue was taken up in ethyl acetate, filtered again through filter earth, washed with ethyl acetate, and concentrated. The residue was washed with hot 2-propanol and concentrated in vacuo.

1. filtrationThe catalyst was filtered off
2. filtrationthrough filter earth
3. washwashed with DCM/ethanol (9:1)
4. concentrationThe filtrate was concentrated
5. customthe solvent was removed firstly with toluene
6. filtrationfiltered again
7. filtrationthrough filter earth
8. washwashed with ethyl acetate
9. concentrationconcentrated
10. washThe residue was washed with hot 2-propanol
11. concentrationconcentrated in vacuo

ORD record

ord-c661cdfec9054074ae9c2eb7bb088696

Source dataset

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08178535B2