p-Toluenesulfonic acid monohydrate → p-Toluenesulfonic acid

HRID 2118645Notes

Reaction equation

HRID 2118645 reaction equation
N1C=CC(CN2CCCNC2=C[N+]([O-])=O)=CC=1.O.[C:19]1([CH3:29])[CH:24]=[CH:23][C:22]([S:25]([OH:28])(=[O:27])=[O:26])=[CH:21][CH:20]=1>CC(C)=O.C(Cl)(Cl)Cl>[CH3:29][C:19]1[CH:24]=[CH:23][C:22]([S:25]([OH:28])(=[O:27])=[O:26])=[CH:21][CH:20]=1

Participants

5

Reactant 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 702494742-(Nitromethylidene)-1-[(pyridin-4-yl)methyl]hexahydropyrimidine

Product 1

HCID 6101p-Toluenesulfonic acidYield 210.4%

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 6212ChloroformSolvent

Procedure

Compound No. 1 (0.73 g) obtained in Example 1 was dissolved in a mixed solvent of acetone (10 ml) and chloroform (50 ml), and p-toluenesulfonic acid hydrate (0.63 g) was added. The mixture was vigorously shaken for 2 hours, and then allowed to stand at room temperature for 3 hours. The precipitated crystals were collected by filtration, and fully washed with acetone to give the p-toluenesulfonate (1.2 g) of compound No. 1 of this invention. mp. 170°-176° C.

Workup

  1. additionwas added
  2. waitto stand at room temperature for 3 hours
  3. filtrationThe precipitated crystals were collected by filtration
  4. washfully washed with acetone

Sources & evidence

ORD record
ord-320b7e5e8b3245f3bef16df40e9ff193
Source dataset
uspto-grants-1987_07
Patent number
US04680294

Reaction notes

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