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ChemicalBook CAS DataBase List 5,6-dichloropyridazin-4-amine

5,6-dichloropyridazin-4-amine synthesis

5synthesis methods
-

Yield: 25%

Reaction Conditions:

with ammonia in tetrahydrofuran at 125; for 5 h;Sealed tube;

Steps:

18.2 Step 2) 5,6-dichloropyridazin-4-amine
A mixture of 3,4,5-trichloropyridazine (17.79 g, 96.99 mmol) and a solution of NH3 in THF ( 250 mL, 750 mmol, 3 M) was stirred at 125 °C in a sealed tube for 5 h. The reaction mixture was concentrated in vacuo and the residue was purified by silica gel column chromatography (EtOAc/PE (v/v) = 1/2) to give the title compound as a white solid (4.01 g, yield 25%).MS (ESI, pos. ion) m/z: 164.1 [M+H]+;1H NMR (600 MHz, CDCb) d (ppm): 8.60 (s, 1H), 4.89 (s, 2H).

References:

SUNSHINE LAKE PHARMA CO., LTD.;CALITOR SCIENCES, LLC;XI, Ning;LI, Minxiong;PENG, Ju;LI, Xiaobo;ZHANG, Tao;HU, Haiyang;CHEN, Wuhong;BAI, Changlin;KE, Donghua;CHEN, Peng WO2019/99311, 2019, A1 Location in patent:Paragraph 000420