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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
The crude diaminoresorcinol (57.0 g), from Step A, containing the Pd/C catalyst, is dissolved in 400 g of 6% aqueous HCl at 80° C. The catalyst is removed by filtration. An additional 50.0 g of concentrated HCl containing 1.5 g of stannous chloride dihydrate is added to the diaminoresorcinol mixture along with 5.0 g of activated carbon. The solution is heated at reflux for 15 minutes and then the carbon is removed by filtration. The filtrate is cooled to 0° C. to allow crystallization of the product. The resulting white precipitate is isolated by filtration under a purge of dry nitrogen. This filter cake is then dried in vacuo at 40° C. to a constant weight to yield 48.7 g of essentially pure (99.8%) 4,6-diaminoresorcinol dihydrochloride having a m.p. of >300° C. Elemental Anal. calc'd for C6H10Cl2N2O2 (213.0643): C, 33.82; H, 4.73; Cl, 33.28; N, 13.15; 0, 15.02, found: C, 33.6; H, 4.64; N, 13.20.
WORKUP
后处理
- customThe catalyst is removed by filtration
- additionAn additional 50.0 g of concentrated HCl containing 1.5 g of stannous chloride dihydrate is added to the diaminoresorcinol mixture along with 5.0 g of activated carbon
- temperatureThe solution is heated
- temperatureat reflux for 15 minutes
- customthe carbon is removed by filtration
- customcrystallization of the product
- customThe resulting white precipitate is isolated by filtration under
- customa purge of dry nitrogen
- customThis filter cake is then dried in vacuo at 40° C. to a constant weight