HRID2387220

反应详情

EQUATION

反应方程式

HRID 2387220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

7-Methyl-pteridine-2,4-diol (prepared by the procedure of ‘Synthesis of 2,6-Disubstituted pyrazines and Related Derivates’, Sharefkin, D. M. J. Am. Chem. Soc., 1959, 345) (4 g, 22.5 mmol) is suspended in a solution of NaOH (2.17 g, 53 mmol) in H2O (20 ml), in an autoclave, and the mixture is heated to 150° C. for 3 days. The reaction mixture is cooled to room temperature and the pH is adjusted to 2.5 by the slow addition of 6M HCl (98 ml). The resulting suspension is cooled in a fridge for 1.5 hours, and the solid is then collected by filtration, washed with cold H2O, and MeOH, and dried in vacuo to yield 3-amino-5-methyl-pyrazin-2-carboxylic acid as a beige solid. [M+H]+ 154

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. temperatureThe resulting suspension is cooled in a fridge for 1.5 hours
  3. filtrationthe solid is then collected by filtration
  4. washwashed with cold H2O, and MeOH
  5. customdried in vacuo