HRID1399583

反应详情

EQUATION

反应方程式

HRID 1399583 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 methyl 2-(2-(cyclohexyl(methyl)amino)-4-methyl-6-p-tolylpyrimidin-5-yl)pentanoate (61 mg; 0.15 mmol) in methanol (1.5 mL) was added a 10 N sodium hydroxide solution (149 μL; 1.489 mmol) and the mixture was heated at 100° C. for 18 h. The volatiles were removed under reduced pressure and the mixture was acidified by adding 6N hydrochloric acid. The suspension was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulphate and concentrated under reduced pressure. The compound was precipitated from a mixture of ethyl acetate and heptane and the formed solid was triturated with heptane to give 40 mg (68%) of the title compound as a white solid. ESI/APCI(+): 396 (M+H). ESI/APCI(−): 350 (M−CO2H); 394 (M−H).

WORKUP

后处理

  1. customThe volatiles were removed under reduced pressure
  2. additionby adding 6N hydrochloric acid
  3. extractionThe suspension was extracted twice with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated under reduced pressure
  7. customThe compound was precipitated from a mixture of ethyl acetate and heptane
  8. customthe formed solid was triturated with heptane