Ammonia → 3,6-Dichloropyridazin-4-amine

A MW vial was charged with 3,4,6-trichloropyridazine (5 g, 27.3 mmol) and 7N NH3 in MeOH (19.47 mL, 136 mmol). The MW vial was sealed and the resulting mixture was submitted to MW irradiation at 100° C. for 30 min. The reaction was cooled down to RT and concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (hexane/EtOAc 35-60%) to afford the title product (1.49 g, 8.63 mmol, 32% yield) as yellow solid. tR: 1.61 min (HPLC 1); tR: 0.45 min (LC-MS 2); ESI-MS: 163 [M+H]+ (LC-MS 2); Rf=0.40 (hexane/EtOAc 1:1).

1. customThe MW vial was sealed
2. customthe resulting mixture was submitted to MW irradiation at 100° C. for 30 min
3. concentrationconcentrated under reduced pressure
4. customThe crude product was purified by silica gel column chromatography (hexane/EtOAc 35-60%)

ORD-Eintrag

ord-81b88d32a089456f9c806b5c13026194

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08975417B2