HRID513598
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
- 10 °C
PROCEDURE
实验过程
2-Amino-4-fluoro-N-quinolin-8-yl-benzenesulfonamide (Example Compound 31) (315 mg, 0.99 mmol) was suspended in acetic acid (4 ml) and cooled to 10° C. Tert-butylnitrite (177 μl, 1.49 mmol) was added and the reaction was warmed to room temperature over 10 min. The reaction was quenched water (5 ml) and the resulting solution was concentrated in vacuo. The crude residue was dissolved in acetic acid (2 ml) and irradiated at 120° C. for 10 mins in the microwave. After cooling, the reaction was concentrated in vacuo. The crude residue was purified by preparative HPLC (acidic conditions) to give the title compound (7 mg, 2%).
WORKUP
后处理
- temperaturethe reaction was warmed to room temperature over 10 min
- customThe reaction was quenched water (5 ml)
- concentrationthe resulting solution was concentrated in vacuo
- dissolutionThe crude residue was dissolved in acetic acid (2 ml)
- customirradiated at 120° C. for 10 mins in the microwave
- temperatureAfter cooling
- concentrationthe reaction was concentrated in vacuo
- customThe crude residue was purified by preparative HPLC (acidic conditions)