HRID547379

反应详情

EQUATION

反应方程式

HRID 547379 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of methyl 3-hydroxy-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-2-carboxylate in 1,4,-dioxane was added dichloro-dicyano benzoquinone (1.1 eqs.). The mixture was stirred and heated to 60° C. for 1 hour. TEA (5 eqs.) was added and stirring was continued for 4 hours. The solution was cooled to room temperature and the product was purified by preparative RP-HPLC, using water (0.1% TFA) and acetonitrile (0.1% TFA) as eluants (column: C18). The product was obtained after lyophilization of the pooled product fractions as a fluffy white material.

WORKUP

后处理

  1. additionTEA (5 eqs.) was added
  2. stirringstirring
  3. temperatureThe solution was cooled to room temperature
  4. customthe product was purified by preparative RP-HPLC
  5. customThe product was obtained after lyophilization of the pooled product fractions as a fluffy white material