Hydrazine hydrate (1:1) → 6-Chloro-3-hydrazinylpyridazin-4-amine

Temperatur

100 °C

To a stirred suspension of 3,6-dichloropyridazin-4-amine (Step 112.1) (1.49 g, 9.09 mmol) in EtOH (15 mL) was added hydrazine hydrate (11.04 mL, 227 mmol) and the resulting mixture was heated up and stirred at 100° C. for 3 hr. The reaction was cooled down to RT and concentrated under reduced pressure. The crude product was triturated with water (25 mL) to afford the title product (478 mg, 3 mmol, 33% yield) as yellow solid. tR: 0.24 min (LC-MS 2); ESI-MS: 160 [M+H]+ (LC-MS 2); ESI-MS: 158 [M−H]− (LC-MS 2).

1. temperaturethe resulting mixture was heated up
2. temperatureThe reaction was cooled down to RT
3. concentrationconcentrated under reduced pressure
4. customThe crude product was triturated with water (25 mL)

ORD-Eintrag

ord-fe5ad3ee10bd4892b72eb56e37fdebf1

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08975417B2