Potassium Carbonate → HCID 20203315, compound

HRID 978472Notes

Reaction equation

HRID 978472 reaction equation
Cl.[CH3:2][O:3][NH2:4].C(=O)([O-])[O-:6].[K+].[K+].[C:11]([C:13]1[CH:21]=[CH:20][C:16]([C:17](Cl)=[O:18])=[CH:15][CH:14]=1)#[N:12]>>[CH3:2][O:3][N:4]([C:17](=[O:18])[C:16]1[CH:20]=[CH:21][C:13]([C:11]#[N:12])=[CH:14][CH:15]=1)[OH:6]

Participants

4

Reactant 3

HCID 11430Potassium CarbonateHCID 801724-Cyanobenzoyl chlorideHCID 521874O-Methylhydroxylamine hydrochloride

Product 1

HCID 20203315HCID 20203315, compound

Procedure

A mixture of 29.4 g (0.350 moles) methoxyaminehydrochloride and 50 g (0.36 moles) potassium carbonate in about 200 ml ice water was stirred, maintaining the temperature below -5° C. until the reactants were dissolved. To that solution, 50 g (0.302 moles) 4-cyano-benzoylchloride were dropped in slowly, maintaining the temperature of the reaction mixture below 0° C. during the addition. The reaction mixture was stirred overnight. The reaction mixture was suction-filtered. The residue, containing the crude product was dried in a heated vacuum oven and then washed with hexane (about 100 ml) and ether (about 2-3 ml) to give the product an off-white solid.

Workup

  1. temperaturemaintaining the temperature below -5° C. until the reactants
  2. dissolutionwere dissolved
  3. temperaturemaintaining the temperature of the reaction mixture below 0° C.
  4. additionduring the addition
  5. stirringThe reaction mixture was stirred overnight
  6. filtrationThe reaction mixture was suction-filtered
  7. additionThe residue, containing the crude product
  8. customwas dried in a heated vacuum oven
  9. washwashed with hexane (about 100 ml) and ether (about 2-3 ml)
  10. customto give the product an off-white solid

Sources & evidence

ORD record
ord-1e1fdbd32c3d4e65b15063a7ba01ba62
Source dataset
uspto-grants-1987_05
Patent number
US04665093

Reaction notes

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