Acetic Acid → 6-Chloro-3,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazine

Temperatur

115 °C

6-chloro-3-hydrazinyl-4-methylpyridazine (Step 111.1) (721 mg, 4.55 mmol) was dissolved in AcOH (15 mL, 262 mmol) and the resulting mixture was heated up and stirred at 115° C. for 1 hr. The reaction was cooled down to RT, diluted with CH2Cl2 and poured into a saturated aq. NaHCO3 solution. The aq. layer was extracted with CH2Cl2. The combined organic layers were dried over Na2SO4, filtered and concentrated under reduced pressure to afford the title product (752 mg, 3.91 mmol, 84% yield) as grey solid. tR: 0.59 min (LC-MS 2); ESI-MS: 183 [M+H]+ (LC-MS 2).

1. temperaturethe resulting mixture was heated up
2. temperatureThe reaction was cooled down to RT
3. extractionThe aq. layer was extracted with CH2Cl2
4. dry with materialThe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-106a0be2b2bf43a3ab0a6fdcc0b1ced0

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08975417B2