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

HRID 259898

反応式

HRID 259898 の反応式
[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]

参加物

5

反応物 2

HCID 428284-Amino-1-naphthalenecarbonitrileHCID 23668193Sodium Nitrite

生成物 1

HCID 221204294-Cyano-1-hydrazinonaphthalene

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ca00712b26aa46aab8efda27a70432d0
出典データセット
uspto-grants-1996_06
特許番号
US05523455

関連ノート

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