Methanesulfonic Acid → HCID 137194547, compound

HRID 2373157Notes

Reaction equation

HRID 2373157 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.[CH3:23][S:24]([OH:27])(=[O:26])=[O:25]>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:24]([O-:27])(=[O:26])(=[O:25])[CH3:23]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 135398745Olanzapine

Product 1

HCID 137194547HCID 137194547, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent2×

Procedure

To a solution of 5.0 g of olanzapine base in 150 ml acetone was slowly added a solution of 1.53 g of methane sulfonic acid in 50 ml of acetone at room temperature. The mixture was stirred for 1 hour and then overnight at 4° C. Crystals were isolated by filtration, washed with 10 ml of acetone and 20 ml of ether and dried overnight at 40° C. in vacuo. Yield: 6.62 g (95%) as a hemi-acetonate.

Workup

  1. customovernight
  2. customat 4° C
  3. customCrystals were isolated by filtration
  4. washwashed with 10 ml of acetone and 20 ml of ether
  5. customdried overnight at 40° C. in vacuo

Sources & evidence

ORD record
ord-8251015b5a094e0780015678e712eb6f
Source dataset
uspto-grants-2008_12
Patent number
US07459449B2

Reaction notes

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