반응 #56597

ord-c8f077f3186244cda816f1911099ee60

반응 방정식

CN(C)c1ccc(N=Nc2ccc([N+](=O)[O-])cc2)c2ccccc12
1-(4-nitro-phenylazo)-4-(dimethylamino)naphtalene
O.O.O.O.O.O.O.O.O.O=S(=O)([O-])O.[Na+]
sodiumhydrogen sulphate nonahydrate
CO
methanol
CN(C)c1ccc(N=Nc2ccc(N)cc2)c2ccccc12
1-(4-amino-phenylazo)-4-(dimethylamino)naphtalene

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도at reflux for 3 h
  3. 3
    여과The brownish precipitate was filtered off
  4. 4
    세척washed with water (200 ml) and cold methanol-water (100 ml/100 ml)

실험 절차

A mixture of 15 g of 1-(4-nitro-phenylazo)-4-(dimethylamino)naphtalene, 75 ml sodiumhydrogen sulphate nonahydrate (50% wt in water) and 80 ml of methanol was heated at reflux for 3 h. The reaction mixture was then cooled to room temperature and poured into 300 ml of water. The brownish precipitate was filtered off, washed with water (200 ml) and cold methanol-water (100 ml/100 ml) to give 12 g of nearly pure 1-(4-amino-phenylazo)-4-(dimethylamino)naphtalene as a brownish solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07419620B2uspto-grants-2008_09