Water → HCID 131710958, compound

HRID 460993Notes

Reaction equation

HRID 460993 reaction equation
[Na+:1].[Na+].[O:3]([C:30]1[CH:35]=[CH:34][C:33]([N:36]=[N:37][C:38]2[C:47]([NH2:48])=[CH:46][CH:45]=[C:44]3[C:39]=2[CH:40]=[CH:41][C:42]([S:49]([O-:52])(=[O:51])=[O:50])=[CH:43]3)=[CH:32][C:31]=1[N+:53]([O-])=O)[C:4]1[CH:9]=[CH:8][C:7]([N:10]=[N:11][C:12]2[C:21]([NH2:22])=[CH:20][CH:19]=[C:18]3[C:13]=2[CH:14]=[CH:15][C:16]([S:23]([O-:26])(=[O:25])=[O:24])=[CH:17]3)=[CH:6][C:5]=1[N+:27]([O-])=O.O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+].O>C(O)(=O)C>[Na+:1].[Na+:1].[O:3]([C:30]1[CH:35]=[CH:34][C:33]([N:36]=[N:37][C:38]2[C:47]([NH2:48])=[CH:46][CH:45]=[C:44]3[C:39]=2[CH:40]=[CH:41][C:42]([S:49]([O-:52])(=[O:51])=[O:50])=[CH:43]3)=[CH:32][C:31]=1[NH2:53])[C:4]1[CH:9]=[CH:8][C:7]([N:10]=[N:11][C:12]2[C:21]([NH2:22])=[CH:20][CH:19]=[C:18]3[C:13]=2[CH:14]=[CH:15][C:16]([S:23]([O-:26])(=[O:25])=[O:24])=[CH:17]3)=[CH:6][C:5]=1[NH2:27]

Participants

5

Reactant 3

HCID 962WaterHCID 73972Sodium sulfide nonahydrateHCID 131710959HCID 131710959, compound

Product 1

HCID 131710958HCID 131710958, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture of 4.0 g. of 5,5'-[oxybis(2-nitro-p-phenyleneazo)]bis-[6-amino-2-naphthalenesulfonic acid] disodium salt and 4.0 g. of sodium sulfide nonahydrate is dissolved in 50 ml. of water by heating on a steam bath for 15 minutes. The solution is cooled and 1.6 ml. of acetic acid is added. The mixture is then filtered through diatomaceous earth. The product is salted out of the filtrate with 25 g. of sodium acetate trihydrate at room temperature, filtered and washed with a small amount of 33% aqueous solution of sodium acetate trihydrate then with ethanol and ether. The product is dissolved in 30 ml. of hot water and filtered through diatomaceous earth. An 18 g. portion of sodium acetate trihydrate is added to the filtrate and this mixture is filtered and the product is washed with ethanol and ether to give 5,5'-[oxybis(2-amino-p-phenyleneazo)]bis-[6-amino-2-naphthalenesulfonic acid] disodium salt.

Workup

  1. additionA mixture of 4.0 g
  2. temperatureThe solution is cooled
  3. filtrationThe mixture is then filtered through diatomaceous earth
  4. filtrationof sodium acetate trihydrate at room temperature, filtered
  5. washwashed with a small amount of 33% aqueous solution of sodium acetate trihydrate
  6. dissolutionThe product is dissolved in 30 ml
  7. filtrationof hot water and filtered through diatomaceous earth
  8. additionportion of sodium acetate trihydrate is added to the filtrate
  9. filtrationthis mixture is filtered
  10. washthe product is washed with ethanol and ether

Sources & evidence

ORD record
ord-08d6a73936db407ea91db3ef166edd90
Source dataset
uspto-grants-1977_12
Patent number
US04061627

Reaction notes

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