Hydrochloric Acid → 1-Hydrazino-4-nitronaphthalene hydrochloride

HRID 1081440노트

반응식

HRID 1081440 반응식
[N:1]([O-])=O.[Na+].[N+:5]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([NH2:18])=[CH:10][CH:9]=1)([O-:7])=[O:6].[ClH:19]>O.CC(O)=O>[ClH:19].[NH:18]([C:11]1[C:12]2[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:8]([N+:5]([O-:7])=[O:6])=[CH:9][CH:10]=1)[NH2:1]

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid3회HCID 130574-Nitro-1-naphthylamineHCID 23668193Sodium Nitrite

생성물 1

HCID 233646151-Hydrazino-4-nitronaphthalene hydrochloride

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
-15 °C

실험 절차

A solution of 1.9 g of sodium nitrite in 10 ml of water is added to a suspension, cooled to -5° C., of 5.2 g of 4-nitro-1-naphthylamine in 150 ml of concentrated HCl, 100 ml of 1N HCl and 150 ml of AcOH. The mixture is left stirring for 1 hour 15 minutes at a temperature of between -5° C. and 0° C. It is cooled to -15° C., and a solution of 12.5 g of stannous chloride dihydrate in 30 ml of concentrated HCl is added very slowly. The temperature is allowed to rise to RT and the reaction mixture is kept stirring for 2 hours 30 minutes. It is filtered, the solid is then taken up with water and the mixture is filtered again. 5.9 g of the expected product are obtained.

후처리

  1. waitThe mixture is left
  2. customto rise to RT
  3. stirringthe reaction mixture is kept stirring for 2 hours 30 minutes
  4. filtrationIt is filtered
  5. filtrationthe mixture is filtered again

출처 및 근거

ORD 기록
ord-ce17f669ae1748a798ba42c9deef67f6
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05585497

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