HRID1030515
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureto reflux for 1.5 h
- temperatureThe resulting mixture was then cooled
- washwashed with 10% sodium carbonate solution
- dry with materialdried (Na2SO4)
- customevaporated to dryness in vacuo
- customThe residue was recrystallized from acetonitrile