HRID2366202

反应详情

EQUATION

反应方程式

HRID 2366202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of pyrimidine-4,6-diamine (500 mg, 4.55 mmol) in dioxane (20 mL) was added acetic anhydride (465 mg, 4.55 mmol) and the resulting mixture was heated under reflux for 15 hours. The reaction was cooled to room temperature and the resulting precipitate was collected by filtration. The filtercake was dissolved in 1N HCl and the pH of the aqueous phase adjusted to 7 by the addition of 1N NaOH. The resulting white precipitate was collected by filtration and dried to afford the desired product as a white solid (420 mg, 61% yield). LCMS (ESI) m/z: 152.0 [M+H+].

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 15 hours
  3. filtrationthe resulting precipitate was collected by filtration
  4. dissolutionThe filtercake was dissolved in 1N HCl
  5. additionthe pH of the aqueous phase adjusted to 7 by the addition of 1N NaOH
  6. filtrationThe resulting white precipitate was collected by filtration
  7. customdried