HRID462523

反应详情

EQUATION

反应方程式

HRID 462523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 360 mg. of sodium in 100 ml. of absolute ethanol was treated with 2.8 g. of guanidine carbonate and 2.0 g. of 4-(3-anilino-2-cyano-allyl)-2,6-dimethoxy carbanilic acid ethyl ester and boiled under reflux for 20 hours. The solution was diluted with 100 ml. of water and the alcohol removed under vacuum. After standing at room temperature for 1 hour, the precipitate was removed by filtration with suction, washed with water and dissolved in about 200 ml. of boiling ethanol. The solution was chromatographed on 100 g. of silica gel using ethanol/ethyl acetate (1:1) and there was obtained 4-[(2,4-diamino-5-pyrimidinyl)-methyl]-2,6-dimethoxy-carbanilic acid ethyl ester which, after recrystallization from ethanol, had a melting point of 228° C. (decomposition).

WORKUP

后处理

  1. temperatureunder reflux for 20 hours
  2. additionThe solution was diluted with 100 ml
  3. customof water and the alcohol removed under vacuum
  4. customthe precipitate was removed by filtration with suction
  5. washwashed with water
  6. dissolutiondissolved in about 200 ml
  7. customThe solution was chromatographed on 100 g