HRID1030515

反应详情

EQUATION

反应方程式

HRID 1030515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-benzyloxy-1,2-diaminobenzene 1.6 g (0.0073 mol) and formic acid (2.6 g, 0.057 mol) was heated to reflux for 1.5 h. The resulting mixture was then cooled, dissolved in methylene chloride, washed with 10% sodium carbonate solution, dried (Na2SO4) and evaporated to dryness in vacuo. The residue was recrystallized from acetonitrile to give the title compound in 0.75 g (46%) yield, m.p. 165°-167° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 1.5 h
  3. temperatureThe resulting mixture was then cooled
  4. washwashed with 10% sodium carbonate solution
  5. dry with materialdried (Na2SO4)
  6. customevaporated to dryness in vacuo
  7. customThe residue was recrystallized from acetonitrile