HRID513598

反应详情

EQUATION

反应方程式

HRID 513598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe reaction was warmed to room temperature over 10 min
  2. customThe reaction was quenched water (5 ml)
  3. concentrationthe resulting solution was concentrated in vacuo
  4. dissolutionThe crude residue was dissolved in acetic acid (2 ml)
  5. customirradiated at 120° C. for 10 mins in the microwave
  6. temperatureAfter cooling
  7. concentrationthe reaction was concentrated in vacuo
  8. customThe crude residue was purified by preparative HPLC (acidic conditions)