Hydrazine hydrate (1:1) → 3-Amino-6-bromopyrazine-2-carbohydrazide

Temperatur

70 °C

To a suspension of methyl 3-amino-6-bromo-pyrazine-2-carboxylate (2.5 g, 10.8 mmol) in ethanol (50 mL) was added hydrazine hydrate (3.2 g, 3 mL, 64.6 mmol) and the reaction mixture heated at 70° C. for 1.5 hours forming a thick yellow solid. The reaction mixture was filtered and the solid washed with water (20 mL) and ethanol (40 mL). The solid was dried in vacuo to yield 3-amino-6-bromo-pyrazine-2-carbohydrazide (2.7 g, 94% yield) as a light yellow solid. 1H NMR (400 MHz, DMSO-d6) δ 4.53 (d, J=3.5 Hz, 2H), 7.62 (s, 2H), 8.31 (s, 1H) and 9.78 (s, 1H) ppm; LC/MS m/z 233.1 [M+H]+

1. customforming a thick yellow solid
2. filtrationThe reaction mixture was filtered
3. washthe solid washed with water (20 mL) and ethanol (40 mL)
4. customThe solid was dried in vacuo

ORD-Eintrag

ord-c7d11d12c78e44348eec3716bdd22687

Quelldatensatz

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08877759B2