HRID1593767

反应详情

EQUATION

反应方程式

HRID 1593767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide (738 mg, 2.84 mmol) in 100 mL of isopropanol was added 3-(3-chloropropoxy)-4-methoxyaniline (611 mg, 2.84 mmol). This mixture was heated to reflux and triethylorthoformate (3.0 mL, 18.0 mmol) was added dropwise. The reaction mixture was heated at reflux overnight. The mixture was filtered while still warm and the collected white solid was washed with isopropanol to give 610 mg of 3-(3-chloropropoxy)-4-methoxyanilino-N-(2,4-dichloro-5-methoxyphenyl)-2-cyano-2-propenamide, mp 185-192° C.; MS (ES) m/z 482.1, 484.2, 486.0 (M−H)−

WORKUP

后处理

  1. temperatureThis mixture was heated
  2. temperatureto reflux
  3. temperatureThe reaction mixture was heated
  4. temperatureat reflux overnight
  5. filtrationThe mixture was filtered
  6. temperaturewhile still warm
  7. washthe collected white solid was washed with isopropanol