4-Amino-1-naphthalenecarbonitrile → 4-Cyano-1-hydrazinonaphthalene

HRID 259898

반응식

HRID 259898 반응식
[N:1]([O-])=O.[Na+].[C:5]([C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([NH2:17])=[CH:9][CH:8]=1)#[N:6]>O.Cl>[C:5]([C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([NH:17][NH2:1])=[CH:9][CH:8]=1)#[N:6]

참가 물질

5

반응물 2

HCID 428284-Amino-1-naphthalenecarbonitrileHCID 23668193Sodium Nitrite

생성물 1

HCID 221204294-Cyano-1-hydrazinonaphthalene

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

A solution of 4.09 g of sodium nitrite in 30 ml of water is added to a solution, cooled to 0° C., of 8.35 g of 4-cyano-1-naphthylamine in 180 ml of 1N HCl. The mixture is left stirring for 1 hour 15 minutes at 0° C. It is cooled to -10° C., and a solution of 41.75 g of stannous chloride dihydrate in 42 ml of concentrated HCl is added slowly. The reaction mixture is stirred for 1 hour, allowing the temperature to rise to RT. It is filtered. The residue is suspended in water and 20 ml of concentrated NaOH are added. The expected product is obtained after filtration, rinses with water and then drying under vacuum, m=8.6 g.

후처리

  1. waitThe mixture is left
  2. temperatureIt is cooled to -10° C.
  3. stirringThe reaction mixture is stirred for 1 hour
  4. customto rise to RT
  5. filtrationIt is filtered
  6. addition20 ml of concentrated NaOH are added

출처 및 근거

ORD 기록
ord-ca00712b26aa46aab8efda27a70432d0
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05523455

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