HRID227025

反应详情

EQUATION

反应方程式

HRID 227025 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

14.9 g (38.5 mmol) of 1-(6-bromo-pyridin-2-ylmethyl)-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid ethyl ester was dissolved/suspended in 300 mL of a 1:1 methanol-water mixture. 1.11 g (46.2 mmol) of lithium hydroxide was added and the mixture was heated up to 65° C. and stirred overnight. The mixture was cooled down to r.t., 300 mL of methanol and 4 mL of concentrated aqueous HCl were added and the solids were filtered off. The solids were then dissolved/suspended in 300 mL ethanol, brought to reflux, cooled down to rt, filtered, washed with 50 mL diethyl ether and dried to yield 9.5 g of the product as a white solid.

WORKUP

后处理

  1. temperatureThe mixture was cooled down to r.t.
  2. filtrationthe solids were filtered off
  3. temperatureto reflux
  4. temperaturecooled down to rt
  5. filtrationfiltered
  6. washwashed with 50 mL diethyl ether
  7. customdried