HRID1074310

反应详情

EQUATION

反应方程式

HRID 1074310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 130 g of 1,5-dihydroxynaphthalene (98.1% strength by weight=0.8 mol), 102 g of ammonia (6.0 mol), 52 ml of ammonium bisulphite solution (490 g of SO2 per liter=0.4 mol) and 449 g of water is heated with stirring to 155° C. in a 1.3 liter titanium autoclave and is stirred at this temperature for 4 hours. 102 g of 50% strength by weight sodium hydroxide solution (1.28 mol of NaOH) are then pumped in with stirring at 155° C. The reaction mixture is cooled to 70° C. and is stirred for a further hour at this temperature. The precipitated 1,5-diaminonaphthalene is then filtered off and washed several times with water at 70° C. Drying in vacuo gives 110 g of 1,5-diaminonaphthalene (=86% of theory, relative to 1,5-dihydroxynaphthalene employed).

WORKUP

后处理

  1. temperatureis heated
  2. stirringwith stirring at 155° C
  3. stirringis stirred for a further hour at this temperature
  4. filtrationThe precipitated 1,5-diaminonaphthalene is then filtered off
  5. washwashed several times with water at 70° C
  6. customDrying in vacuo