反应 #806304

ord-1cbf5cb58a3f420389ba7b092e4888e9

反应条件

温度
-10°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction vessel was cooled to 0° C. before the stopper
  2. 2
    其他was removed
  3. 3
    其他to remove excess hydrogen chloride gas
  4. 4
    其他The solvent was evaporated
  5. 5
    其他the residue was triturated in diethyl ether (100 mL)

实验过程

Hydrogen chloride gas was passed through a solution of 2-ethoxy-4-methoxy-benzonitrile (6.3 g, 35.55 mmol) in anhydrous ethanol (70 mL) cooled to −10° C. After 30 min, hydrogen chloride gas was stopped and the reaction mixture was stirred at room temperature in a closed reaction vessel for 4 d. The reaction vessel was cooled to 0° C. before the stopper was removed. Argon gas was passed through the solution to remove excess hydrogen chloride gas. The solvent was evaporated and the residue was triturated in diethyl ether (100 mL) to afford ethyl 2-ethoxy-4-methoxy-benzimidate hydrochloride (7.3 g, 79%). It was used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07132421B2uspto-grants-2006_11