HRID395399

反应详情

EQUATION

反应方程式

HRID 395399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2 g (0.0069 mol) of methyl 2,6-bis(trifluoromethyl)-4-hydroxy-3-pyridinecarboxylate (example 4 of U.S. Pat. No. 4,655,816) in 20 mL of acetonitrile was added 0.7 g of triethylamine. A solution of 1.6 g (0.0069 mol) of diphenylcarbamyl chloride in 20 mL of acetonitrile was added to the above mixture and the resulting mixture was stirred at room temperature over the weekend. The precipitate formed was filtered off and the filtrate was concentrated in vacuo. The residue was slurried with ether. The insoluble material was filtered. The ether filtrate was concentrated and the residue was recrystallized from cyclohexane to give a white solid, mp 114-116° C.

WORKUP

后处理

  1. customThe precipitate formed
  2. filtrationwas filtered off
  3. concentrationthe filtrate was concentrated in vacuo
  4. filtrationThe insoluble material was filtered
  5. concentrationThe ether filtrate was concentrated
  6. customthe residue was recrystallized from cyclohexane
  7. customto give a white solid, mp 114-116° C.