HRID215959
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
Potassium phosphate (0.017 g, 0.078 mmol) in water (0.10 mL) was added to a mixture of 8-(5-bromo-3-chloropyridin-2-yl)-2-(cis-4-hydroxycyclohexyl)-2,8-diazaspiro[4.5]decan-1-one (11.6 mg, 0.0262 mmol), 3-[(methylamino)carbonyl]phenylboronic acid (7.0 mg, 0.039 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.9 mg, 0.0008 mmol) in 1,4-dioxane (0.78 mL). The resulting mixture was heated and stirred at 120° C. for 2 h. The mixture was diluted with ethyl acetate and washed with water and brine. The organic layer was dried over Na2SO4, filtered, concentrated under reduced pressure. The residue was purified by Prep-HPLC to afford the desired product. LCMS: (M+H)+=497.1/499.1.
WORKUP
后处理
- temperatureThe resulting mixture was heated
- washwashed with water and brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by Prep-HPLC