Oxalic Acid → HCID 86692190, compound

HRID 536601Notes

Reaction equation

HRID 536601 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-0325d22181db4142a5b953d1adb21060
Source dataset
uspto-grants-2014_10
Patent number
US08859610B2

Reaction notes

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