反应详情

温度

85 °C

A mixture of 6-aminopyridazin-3-ol (2 g, 18.00 mmol), NaOH (0.720 g, 18.00 mmol) and MeI (1.126 mL, 18.00 mmol) was stirred for 2.5 hr at 85° C. under Ar. The reaction mixture was concentrated. The crude material was purified by silica gel column chromatography (NH3 1%/CH2Cl2/MeOH 4-7%) to afford the title product (538 mg, 4.30 mmol, 24% yield) as a yellow solid. tR: 0.25 min (LC-MS 2); ESI-MS: 126 [M+H]+ (LC-MS 2); Rf=0.36 (CH2Cl2/MeOH 9:1).

1. concentrationThe reaction mixture was concentrated
2. customThe crude material was purified by silica gel column chromatography (NH3 1%/CH2Cl2/MeOH 4-7%)