反応 #1161492

反応方程式

sodium hydroxide

1,5-dihydroxynaphthalene

ammonia

ammonium bisulphite

→

1,5-diaminonaphthalene

収率 173.8%

溶媒

water

反応条件

後処理

1. 1
   温度is heated
2. 2
   workup.STIRRINGwith stirring at 155° C
3. 3
   workup.STIRRINGis stirred for a further hour at this temperature
4. 4
   ろ過The precipitated 1,5-diaminonaphthalene is then filtered off
5. 5
   洗浄washed several times with water at 70° C
6. 6
   その他Drying in vacuo

実験手順

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).

出典