HRID421888

反应详情

EQUATION

反应方程式

HRID 421888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
62.5 °C

PROCEDURE

实验过程

Preparation of 2-(4-bromo-2-fluorophenylamino)-6-methoxynicotinic acid methyl ester: To a mixture of 2-(4-bromo-2-fluorophenylamino)-6-chloronicotinic acid methyl ester (2.00 g, 5.56 mmol) and sodium methoxide (0.791 g, 13.9 mmol) was added MeOH (50 mL) to give a slurry that was stirred at 60-65° C. for 16 hours under N2. Additional sodium methoxide (0.791 g, 13.9 mmol) was added and the reaction mixture was allowed to stir another 3 days at 60-65° C. The reaction mixture was cooled to room temperature and glacial acetic acid was added dropwise until the pH was 7. The resulting suspension was filtered and washed with H2O to yield a pink solid that was collected and dried under vacuum to yield 1.74 g (88%) pure desired product.

WORKUP

后处理

  1. customto give a slurry that
  2. stirringto stir another 3 days at 60-65° C
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationThe resulting suspension was filtered
  5. washwashed with H2O
  6. customto yield a pink solid
  7. customthat was collected
  8. customdried under vacuum