HRID463621

反应详情

EQUATION

反应方程式

HRID 463621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred suspension of 1.4 g of 2-amino-4-methoxy-6-methylpyrimidine in 20 ml of dry acetonitrile at room temperature was added 2.2 g of 2-chloropyridine-3-sulfonylisocyanate. The mixture was stirred for several hours and filtered. Evaporation of the filtrate yielded a solid residue which was stirred in approximately 30 ml of water while adjusting the pH of this mixture to 11 by the addition of 10% of NaOH. This solution was filtered, the filtrate pH adjusted to pH 7 by adding 10% hydrochloric acid and the resulting neutral solution was again filtered. The desired product was then precipitated from this filtrate by adjusting the pH to 2, collected in a sintered funnel and dried in a vacuum oven at room temperature. It melted at 165°-168°.

WORKUP

后处理

  1. filtrationfiltered
  2. customEvaporation of the filtrate
  3. customyielded a solid residue which
  4. filtrationThis solution was filtered
  5. additionby adding 10% hydrochloric acid
  6. filtrationthe resulting neutral solution was again filtered
  7. customThe desired product was then precipitated from this filtrate
  8. customcollected in a sintered funnel
  9. customdried in a vacuum oven at room temperature