Sulfuric Acid → HCID 12573606, compound

HRID 2286351Notes

Reaction equation

HRID 2286351 reaction equation
[C:1]1([S:11]([O-:14])(=[O:13])=[O:12])[CH:6]=[CH:5][CH:4]=[C:3]([S:7]([O-:10])(=[O:9])=[O:8])[CH:2]=1.[Na+:15].[Na+].S(=O)(=O)(O)O.[N+:22]([O-])([O-:24])=[O:23].[Na+]>>[N+:22]([C:5]1[CH:6]=[C:1]([S:11]([O-:14])(=[O:13])=[O:12])[CH:2]=[C:3]([S:7]([O-:10])(=[O:9])=[O:8])[CH:4]=1)([O-:24])=[O:23].[Na+:15].[Na+:15]

Participants

4

Reactant 3

HCID 1118Sulfuric AcidHCID 24268Sodium NitrateHCID 71577Disodium benzene-1,3-disulfonate

Product 1

HCID 12573606HCID 12573606, compound

Conditions

Temperature
65 °C

Procedure

A mixture of 141 g. of disodium benzene-1,3-disulfonate in 450 ml. of concentrated sulfuric acid is stirred and heated to 65° C. During the course of 31/4 hours, 120 g. of sodium nitrate are added in portions while the mixture is stirred and maintained at 70° C. After addition is complete, the mixture is cooled to 5° C. and 900 g. of ice are added with stirring. The mixture is filtered overnight with vaccum. The cake is warmed on a steam bath in 250 ml. of hot water, filtered and washed with hot water. The combined filtrate and wash is cooled to 5° C. and the resulting crystals are collected by filtration giving disodium 5-nitrobenzene-1,3-disulfonate.

Workup

  1. additionA mixture of 141 g
  2. temperaturemaintained at 70° C
  3. additionAfter addition
  4. temperaturethe mixture is cooled to 5° C.
  5. additionof ice are added
  6. stirringwith stirring
  7. filtrationThe mixture is filtered overnight with vaccum
  8. temperatureThe cake is warmed on a steam bath in 250 ml
  9. filtrationof hot water, filtered
  10. washwashed with hot water
  11. washThe combined filtrate and wash
  12. temperatureis cooled to 5° C.
  13. filtrationthe resulting crystals are collected by filtration

Sources & evidence

ORD record
ord-41ca054f20934343bb3790bcc9100938
Source dataset
uspto-grants-1981_05
Patent number
US04265908

Reaction notes

Loading…