HRID59034

反应详情

EQUATION

反应方程式

HRID 59034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ethyl 4-(4-amino-3-fluorophenoxy)-2-aminopyridin-3-yl-carbamate (6a) (480 mg, 1.6 mmol) was dissolved in dry THF (8 mL) and cooled at 0° C. Sodium hydride (60% in mineral oil, 80 mg, 2.0 mmol) was added, and the reaction mixture was stirred for 40 minutes at 0° C. Methyl iodide (130 μL, 1.8 mmol) was added at 0° C. The ice bath was removed, and the mixture was stirred at room temperature for 18 hours. The solvent was evaporated and the residue partitioned between DCM and distilled water. The organic layer was dried and evaporated, and the residue washed with diethyl ether to afford the title compound as a brown solid.

WORKUP

后处理

  1. customThe ice bath was removed
  2. stirringthe mixture was stirred at room temperature for 18 hours
  3. customThe solvent was evaporated
  4. customthe residue partitioned between DCM
  5. distillationdistilled water
  6. customThe organic layer was dried
  7. customevaporated
  8. washthe residue washed with diethyl ether