HRID10240

反应详情

EQUATION

反应方程式

HRID 10240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of dimethyl-(o-methoxyphenoxy)malonate (10 g) in dry methanol (80 ml) was cooled to 0° C. Sodium methylate (6.71 g) was added portionwise. To the suspension was added of acetamidine hydrochloride (2.84 g) and the mixture was stirred overnight at r.t. The solvent was removed under reduced pressure and the residue was suspended in diethyl ether (100 ml). The solid was filtered off, washed with another portion of diethyl ether (100 ml) and dissolved in water (50 ml). The pH was adjusted to 4 by adding glacial acetic acid (25 ml). The white precipitate that formed was filtered off, washed with water and dried to yield 5-(o-methoxyphenoxy)-4,6-dihydroxy-2-methyl-pyrimidine (5.17 g) (or a tautomer) as a white powder.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. filtrationThe solid was filtered off
  3. washwashed with another portion of diethyl ether (100 ml)
  4. dissolutiondissolved in water (50 ml)
  5. additionby adding glacial acetic acid (25 ml)
  6. customThe white precipitate that formed
  7. filtrationwas filtered off
  8. washwashed with water
  9. customdried