Ammonia → 1,5-Diaminonaphthalene

HRID 1074310

反応式

HRID 1074310 の反応式
O[C:2]1[C:11]2[C:6](=[C:7](O)[CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.[NH3:13].S(=O)(O)[O-].[NH4+:18].[OH-].[Na+]>[Ti].O>[NH2:13][C:2]1[C:11]2[C:6](=[C:7]([NH2:18])[CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 222AmmoniaHCID 67491,5-DihydroxynaphthaleneHCID 14798Sodium HydroxideHCID 10441651Ammonium Bisulfite

生成物 1

HCID 167201,5-Diaminonaphthalene収率 173.8%

試薬・触媒・溶媒 2

HCID 23963Titanium触媒HCID 962Water溶媒

反応条件

温度
70 °C

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).

後処理

  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

出典と根拠

ORDレコード
ord-36f844ae152f4328837bb8c8db81d877
出典データセット
uspto-grants-1990_11
特許番号
US04973758

関連ノート

読み込み中…