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ChemicalBook CAS DataBase List 3,5-dichloropyridazin-4-amine

3,5-dichloropyridazin-4-amine synthesis

3synthesis methods
-

Yield:53180-76-0 36%

Reaction Conditions:

with ammonium hydroxide in ethanol at 120; for 0.416667 h;Microwave irradiation;

Steps:

4 3,5-Dichloropyridazin-4-amine

A mixture of 3,4,5-trichloropyridazine (Preparation 3, 500 mg, 2.73 mmole) in EtOH (5.5 mL) and NH4OH (5.5 mL) was heated under microwave irradiation 120° C. for 25 minutes. Concentration under reduced pressure and purification via silica gel column chromatography eluting with acetone:dichloromethane (0-15% acetone), provided the title product in 36% yield, 163 mg. 1H NMR (400 MHz, CDCl3): δ ppm 5.11 (br s, 2H), 8.74 (s, 1H). LCMS Rt=0.27 minutes MS m/z 164 [M+H]+

References:

US2014/171435,2014,A1 Location in patent:Paragraph 0454; 0455; 0456