HRID2265941

反应详情

EQUATION

反应方程式

HRID 2265941 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

3-(6-Chloro-pyridin-3-yl)-N-(3-fluoro-4-methanesulfonylamino-benzyl)-acrylamide (15 mg, 0.413 mmol) was added to pyrrolidine (0.5 ml) and the mixture was stirred for 12 hrs at 90° C. The resulting residue was dissolved in EtOAc, then washed three times with H2O, and neutralized with 1N HCl to pH 5˜7. The resulting solution was washed with brine, and then dried over anhyd. Na2SO4, filtered and concentrated under reduced pressure. The crude residue was recrystallized (CH2Cl2) to yield the title compound (4 mg, 24%).

WORKUP

后处理

  1. washwashed three times with H2O
  2. washThe resulting solution was washed with brine
  3. customdried over anhyd
  4. filtrationNa2SO4, filtered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude residue was recrystallized (CH2Cl2)