HRID10241

反应详情

EQUATION

反应方程式

HRID 10241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At 5° C. sodium methylate (12.7 g) was added portionwise to a solution of dimethyl-(o-methoxyphenoxy)malonate (18.9 g) in methanol (450 ml). Upon completion of the addition stirring was continued at r.t. for 30 min followed by the addition of formamidine hydrochloride (6 g). The mixture was stirred at r.t. for 72 h. Eventually, the solvent was removed under reduced pressure and the remaining residue was suspended in diethyl ether. The solid material was filtered off and dissolved in water (100 ml). The solution was acidified with conc. hydrochloric acid. A white precipitate formed. The precipitate was collected, washed with water and dried to give 5-(o-methoxyphenoxy)-4,6-dihydroxy-pyrimidine (15.1 g) (or a tautomer) as a white powder.

WORKUP

后处理

  1. additionUpon completion of the addition
  2. stirringThe mixture was stirred at r.t. for 72 h
  3. customEventually, the solvent was removed under reduced pressure
  4. filtrationThe solid material was filtered off
  5. dissolutiondissolved in water (100 ml)
  6. customA white precipitate formed
  7. customThe precipitate was collected
  8. washwashed with water
  9. customdried