Oxalic Acid → HCID 86692190, compound

HRID 1470672Notes

Reaction equation

HRID 1470672 reaction equation
[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[CH3:7][N+:8]1([CH3:29])[CH2:12][CH:11]([O:13][C:14]([C:16]([OH:28])([CH:23]2[CH2:27][CH2:26][CH2:25][CH2:24]2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[O:15])[CH2:10][CH2:9]1.C([O-])(=O)C>CO>[CH3:7][N+:8]1([CH3:29])[CH2:12][CH:11]([O:13][C:14]([C:16]([OH:28])([CH:23]2[CH2:24][CH2:25][CH2:26][CH2:27]2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[O:15])[CH2:10][CH2:9]1.[C:1]([O-:6])(=[O:5])[C:2]([O-:4])=[O:3]

Participants

4

Reactant 2

HCID 971Oxalic AcidHCID 23726014HCID 23726014, compound

Product 1

HCID 86692190HCID 86692190, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Glycopyrrolate oxalate was prepared using process (2) from Example 1. Equimolar amounts of oxalic acid and glycopyrrolate acetate were dissolved in methanol then fast evaporated and dried under vacuum. The resulting glassy, gel-like material was recrystallized by slurrying in ethyl acetate to produce grey solids that were then dried under vacuum before analysis by XRPD and proton NMR spectroscopy. The XRPD pattern can be found in FIG. 16.

Workup

  1. customthen fast evaporated
  2. customdried under vacuum
  3. customThe resulting glassy, gel-like material was recrystallized
  4. customto produce grey solids that
  5. customwere then dried under vacuum before analysis by XRPD and proton NMR spectroscopy

Sources & evidence

ORD record
ord-97e8a9a79301423d8999fba6ee595c9a
Source dataset
uspto-grants-2015_04
Patent number
US09006462B2

Reaction notes

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