Oxalic Acid → HCID 86692190, compound

HRID 1042959Notes

Reaction equation

HRID 1042959 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-a970e49e9b7348218be05bf90c32dac7
Source dataset
uspto-grants-2013_10
Patent number
US08558008B2

Reaction notes

Loading…