Oxalic Acid → HCID 86692190, compound

HRID 1470670Notes

Reaction equation

HRID 1470670 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-2285f460e5444a72b8b23d6b26058473
Source dataset
uspto-grants-2015_04
Patent number
US09006461B2

Reaction notes

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