HRID259812

反应详情

EQUATION

反应方程式

HRID 259812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium hydroxide (18.2 g, 325 mmol) was dissolved in 100 mL of H2O, and 100 mL of methanol was added. 2-Acetyl-6-bromopyridine (65 g, 325 mmol) and (68 g, 650 retool) of p-anisaldehyde were dissolved together in 400 mL of methanol, and the solution was poured into the KOH solution. Precipitation of product began Within a few minutes, and the reaction was allowed to stand at room temperature overnight. The precipitate was collected, washed with isopropanol, and dried to yield 79 g (76%) of the product as a yellow solid, mp 100°-102° C. FDMS (m/e) 317M. An aliquot was purified by column chromatography on Woelm Silica gel, elution with 100% dichloromethane. Anal. Calcd for C15H12BrNO2 : C, 56.63; H, 3.80; N, 4.40. Found: C, 6.66;H, 3.87; N, 4.41. The NMR and IR spectra were consistent with the assigned structure and the product was homogeneous by TLC.

WORKUP

后处理

  1. customPrecipitation of product
  2. waitbegan Within a few minutes
  3. customThe precipitate was collected
  4. washwashed with isopropanol
  5. customdried