HRID1938786

反应详情

EQUATION

反应方程式

HRID 1938786 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 4-pyridine carboxaldehyde (36.7 mL, 0.384 mol) and malonic acid (40g, 0.384 mol) in 31 mL of pyridine was added piperdine (0.12 mL) and the mixture was warmed to 100° C. Caution: large volumes of CO2 evolved. After 0.5 h, the reaction was cooled to room temperature (RT) and the solution solidified. This was triturated with 240 mL of water and filtered, and washed with 2×50 mL portions of water. The solid was dried overnight at 42° C. under vacuum (10 mm Hg) to provide 37.1 g of a white solid; mp 295°-297° C.

WORKUP

后处理

  1. temperaturethe reaction was cooled to room temperature (RT)
  2. customThis was triturated with 240 mL of water
  3. filtrationfiltered
  4. washwashed with 2×50 mL portions of water
  5. customThe solid was dried overnight at 42° C. under vacuum (10 mm Hg)