Hydroxybenzenesulfonic acid → HCID 137194545, compound

HRID 2373155Notes

Reaction equation

HRID 2373155 reaction equation
[CH3:1][C:2]1[S:6][C:5]2[NH:7][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=3[N:14]=[C:15]([N:16]3[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]3)[C:4]=2[CH:3]=1.O.[C:24]1([S:30]([OH:33])(=[O:32])=[O:31])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CC(C)=O>[CH3:1][C:2]1[S:6][C:5]2[NH:7][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=3[N:14]=[C:15]([N:16]3[CH2:17][CH2:18][N:19]([CH3:22])[CH2:20][CH2:21]3)[C:4]=2[CH:3]=1.[S:30]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)([O-:33])(=[O:32])=[O:31]

Participants

4

Reactant 2

HCID 15619088Hydroxybenzenesulfonic acidHCID 135398745Olanzapine

Product 1

HCID 137194545HCID 137194545, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent2×

Procedure

To a solution of 5.0 g of olanzapine in 150 ml acetone was slowly added a solution of 2.8 g benzenesulfonic acid monohydrate in 50 ml acetone at room temperature under stirring. The mixture was stirred 1 hour at room temperature and then at 4° C. overnight. Crystals were isolated by filtration, washed with 20 ml of acetone and 20 ml of ether and dried at 40° C. under vacuum overnight. Yield: 5.98 g (79%).

Workup

  1. stirringThe mixture was stirred 1 hour at room temperature
  2. customat 4° C.
  3. customovernight
  4. customCrystals were isolated by filtration
  5. washwashed with 20 ml of acetone and 20 ml of ether
  6. customdried at 40° C. under vacuum overnight

Sources & evidence

ORD record
ord-87944d1893044a38b325394a0e4d6bf8
Source dataset
uspto-grants-2008_12
Patent number
US07459449B2

Reaction notes

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