HRID1449075

反应详情

EQUATION

反应方程式

HRID 1449075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Into 30 ml of acetonitrile was dissolved 4 g of ethylβ-amino-β-ethoxy acrylate, and 3 g of phenyl isocyanate was added thereto. The resulting solution was allowed to stand at room temperature for 24 hours. Into a mixed solution of 20 ml of methanol, 6 g of triethylamine and 5 ml of glacial acetic acid there was dissolved 4.7 g of p-sulfophenyl hydrazine, and the above solution, in which the esterification reaction had been completed, was added thereto. The resulting solution was allowed to stand at room temperature for 5 days. The crystals obtained were collected, washed with acetonitrile, and then recrystallized from methanol; thus 7.5 g of crystals of a melting point of 240° to 242° C. was obtained.

WORKUP

后处理

  1. additionwas added
  2. customthe above solution, in which the esterification reaction
  3. additionwas added
  4. waitto stand at room temperature for 5 days
  5. customThe crystals obtained
  6. customwere collected
  7. washwashed with acetonitrile
  8. customrecrystallized from methanol