HRID352227

反应详情

EQUATION

反应方程式

HRID 352227 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product was prepared in a manner similar to preparation 396 using the pre-formed sodium salt of the 3-hydroxypyridine (2.13 g; 18.2 mmol; 1.2 equiv) and an aliquot of bromo-pyridin-3-yl-acetic acid ethyl ester (approx. 3.6 g; 15 mmol) in dimethylformamide (20 mL). Column purification over SiO2 (0.5% then 1.5% methanol/chloroform) produced a yellow/orange oil (2.02; approx. 50% yield). MS(ES) calc'd: [M+H]+=259.2 m/z; [M−H]−=257.2 m/z. Found: 259.1 m/z; 257.1 m/z.

WORKUP

后处理

  1. customColumn purification over SiO2 (0.5%
  2. custom1.5% methanol/chloroform) produced a yellow/orange oil (2.02; approx. 50% yield)