Sulfuric Acid → 3-Amino-1,5-naphthalenedisulfonic acid

HRID 838914ノート

反応式

HRID 838914 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([S:18]([OH:21])(=[O:20])=[O:19])[C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([S:14]([OH:17])(=[O:16])=[O:15])[C:12]=2[CH:13]=1)([O-])=O.S(=O)(=O)(O)O.C([O-])=O.[Na+]>[Pd].O>[NH2:1][C:4]1[CH:5]=[C:6]([S:18]([OH:21])(=[O:20])=[O:19])[C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([S:14]([OH:17])(=[O:16])=[O:15])[C:12]=2[CH:13]=1

参加物

6

反応物 3

HCID 1118Sulfuric AcidHCID 670321,5-Naphthalenedisulfonic acid, 3-nitro-HCID 2723810Sodium Formate2 回

生成物 1

HCID 85633-Amino-1,5-naphthalenedisulfonic acid

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

A solution of 20.6 parts of the magnesium salt of 3-nitronaphthalene-1,5-disulphonic acid and 5.5 parts of sulphuric acid in 160 parts of water is reacted with 20.4 parts of sodium formate and 1.24 parts (dry weight) of 3% palladium-on-carbon catalyst according to the procedure of Example 1. After 22 hours a further 10 parts of sodium formate are added and stirring under reflux is continued for an additional period of 20 hours. The mixture is cooled and filtered and the filter cake is washed with dilute sulphuric acid until only the catalyst remains on the filter. Analysis of the combined filtrates by ultraviolet spectroscopy and by titration of an aliquot with sodium nitrite solution indicates that the theoretical yield (17.6 parts) of 3-aminonaphthalene-1,5-disulphonic acid has been formed.

後処理

  1. temperatureunder reflux
  2. temperatureThe mixture is cooled
  3. filtrationfiltered
  4. washthe filter cake is washed with dilute sulphuric acid until only the catalyst

出典と根拠

ORDレコード
ord-9a10cfa3e18a48a693d4047f8b6caea8
出典データセット
uspto-grants-1978_06
特許番号
US04093646

反応ノート

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