Sodium Chloride → HCID 88746855, compound

HRID 261358Notes

Reaction equation

HRID 261358 reaction equation
C1(C)C=CC(=[C:7]2[CH:12]3[C:13]([CH3:15])([CH3:14])[C:9]([CH3:16])([CH2:10][CH2:11]3)[C:8]2=[O:17])CC=1.[OH:19][S:20]([OH:23])(=O)=[O:21].O=S(=O)=O.[Cl-].[Na+:29]>>[CH3:16][C:9]1[CH:10]=[CH:11][C:12]([CH:13]=[C:7]2[CH:12]3[C:13]([CH3:15])([CH3:14])[C:9]([CH3:16])([CH2:10][CH2:11]3)[C:8]2=[O:17])=[CH:7][C:8]=1[S:20]([O-:23])(=[O:21])=[O:19].[Na+:29]

Participants

4

Reactant 3

HCID 5234Sodium ChlorideHCID 24681Fuming sulfuric acidHCID 131711595HCID 131711595, compound

Product 1

HCID 88746855HCID 88746855, compound

Procedure

25.4 g of 3-p-tolylidene camphor are added to 64 ml of oleum containing 10% SO3, with cooling so as to keep the temperature of the reaction mixture around 35° C. The resulting mixture is then poured into 150 ml of a saturated sodium chloride solution, the mixture being cooled to below 25° C. A precipitate is obtained which is filtered and then washed with a saturated sodium chloride solution. The wet product is made into paste in 70 ml of water. It is then filtered and recrystallized in an 80:20 water-acetone mixture. Thus, 29.3 g of a white powder, melting at 240° C. are obtained.

Workup

  1. temperaturewith cooling so as
  2. customthe temperature of the reaction mixture around 35° C
  3. temperaturethe mixture being cooled to below 25° C
  4. customA precipitate is obtained which
  5. filtrationis filtered
  6. washwashed with a saturated sodium chloride solution
  7. filtrationIt is then filtered
  8. customrecrystallized in an 80:20 water-acetone mixture

Sources & evidence

ORD record
ord-e482dfd8acbb4312babac65e0b6137b2
Source dataset
uspto-grants-1979_08
Patent number
US04165336

Reaction notes

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