Potassium Carbonate → HCID 10103167, compound

HRID 266551Notes

Reaction equation

HRID 266551 reaction equation
[CH:1]1([C:4](=[O:9])[CH2:5][C:6](=O)[CH3:7])[CH2:3][CH2:2]1.Cl.[NH2:11]O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH:1]1([C:4]2[O:9][N:11]=[C:6]([CH3:7])[CH:5]=2)[CH2:3][CH2:2]1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 110188691-Cyclopropyl-butane-1,3-dione

Product 1

HCID 10103167HCID 10103167, compoundYield 81.3%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 1-cyclopropylbutan-1,3-dione (65.3 g), hydroxylamine hydrochloride (36.6 g) and anhydrous potassium carbonate (71.8 g) in ethanol (375 ml) was stirred and heated at reflux for 2 hours. The mixture was cooled and filtered and the filtrate was evaporated to dryness. The residue was distilled under reduced pressure to give 5-cyclopropyl-3-methyl isoxazole containing approximately 20% 3-cyclopropyl-5-methylisoxazole (51.85 g) as a clear oil, b.p. 74° C./12 mm.Hg.

Workup

  1. temperatureheated
  2. temperatureat reflux for 2 hours
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. customthe filtrate was evaporated to dryness
  6. distillationThe residue was distilled under reduced pressure

Sources & evidence

ORD record
ord-f97fdec3936b4c2bb6243fb51993638b
Source dataset
uspto-grants-1997_07
Patent number
US05650533

Reaction notes

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