Potassium Carbonate → HCID 19377223, compound

HRID 1975287Notes

Reaction equation

HRID 1975287 reaction equation
C(O)(=O)C(O)=O.[CH2:7]([NH:14][CH2:15][CH2:16][CH2:17][C:18]1[CH:19]=[C:20]([CH:24]=[CH:25][CH:26]=1)[C:21]([NH2:23])=[O:22])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+].[OH-].[K+]>O.C(OCC)(=O)C>[CH2:7]([NH:14][CH2:15][CH2:16][CH2:17][C:18]1[CH:19]=[C:20]([CH:24]=[CH:25][CH:26]=1)[C:21]([NH2:23])=[O:22])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Participants

6

Reactant 3

HCID 11430Potassium CarbonateHCID 14797Potassium HydroxideHCID 19377222HCID 19377222, compound

Product 1

HCID 19377223HCID 19377223, compoundYield 97.6%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8857Ethyl AcetateSolvent

Procedure

To 6.7 g (0.0187 mole) of 3-[3-(benzylamino)propyl]benzamide oxalate (the product of step (g)) slurried in 20 ml water, 7.7 g (0.056 mole) potassium carbonate (and 700 mg potassium hydroxide) in 50 ml ethyl acetate was stirred until all solids were dissolved. The aqueous and ethyl acetate phases were separated. The aqueous layer was washed with about 30 ml ethyl acetate. The ethyl acetate extracts were combined, washed over saturated saline and dried over sodium sulfate, filtered. The filtrate was dried to an oil on a vacuum pump overnight to give 4.9 g of the above-identified product.

Workup

  1. dissolutionwere dissolved
  2. customThe aqueous and ethyl acetate phases were separated
  3. washThe aqueous layer was washed with about 30 ml ethyl acetate
  4. washwashed over saturated saline
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customThe filtrate was dried to an oil on a vacuum pump overnight

Sources & evidence

ORD record
ord-bbcea82981cf49fea14733710d642c8b
Source dataset
uspto-grants-1994_02
Patent number
US05286252

Reaction notes

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