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

HRID 838914노트

반응식

HRID 838914 반응식
[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

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 670321,5-Naphthalenedisulfonic acid, 3-nitro-HCID 2723810Sodium Formate2회

생성물 1

HCID 85633-Amino-1,5-naphthalenedisulfonic acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-9a10cfa3e18a48a693d4047f8b6caea8
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093646

반응 노트

불러오는 중…