反应详情

To a solution of methyl 2-chloro-4-[7-(quinolin-6-ylmethyl)imidazo[1,2-b][1,2,4]triazin-2-yl]benzoate (Step 3, 1.10 g, 2.56 mmol) in tetrahydrofuran (7.0 mL) and methanol (5.0 mL) was added a solution of lithium hydroxide (0.245 g, 10.2 mmol) in water (3.0 mL). The mixture was stirred at room temperature for 2 h. and concentrated under reduced pressure to a volume of about 3 mL. The residue was diluted with water (3 mL), and adjusted with 1N HCl to pH of about 4-5. The precipitate was filtered out, washed several times with water and dried in air overnight. The precipitate was then triturated sequentially with ether and dichloromethane (DCM)-Hexane (1:1). The desired product (638 mg, 60%) was obtained. LCMS (M+H)+: m/z=415.9/417.9.

1. concentrationconcentrated under reduced pressure to a volume of about 3 mL
2. additionThe residue was diluted with water (3 mL)
3. filtrationThe precipitate was filtered out
4. washwashed several times with water
5. customdried in air overnight
6. customThe precipitate was then triturated sequentially with ether and dichloromethane (DCM)-Hexane (1:1)