HRID2060860
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
To a solution of 6-(5-methylnaphthalen-1-yloxy)nicotinonitrile (Preparation 22) (530 mg, 2.04 mmol) in carbon tetrachloride (30 mL) under argon was added N-bromosuccinimide (435 mg, 2.44 mmol) followed by benzoyl peroxide (25 mg, 0.1 mmol). The mixture was heated to 70° C. for 16 h. The reaction mixture was cooled, filtered through celite, and washed with DCM (70 mL). The organic phase was washed with NaHCO3 (30 mL), brine (30 mL) and dried (MgSO4). Solvent was removed in vacuo to give the title compound: RT=3.93 min; m/z (ES+)=341.0 [M+H]+.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- filtrationfiltered through celite
- washwashed with DCM (70 mL)
- washThe organic phase was washed with NaHCO3 (30 mL), brine (30 mL)
- dry with materialdried (MgSO4)
- customSolvent was removed in vacuo