Ammonia → HCID 13081567, compound

HRID 648079Notes

Reaction equation

HRID 648079 reaction equation
[NH3:1].O=O.C[CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C:6]1=[O:11].[CH3:12]O>>[C:5]([CH2:10][CH2:9][CH2:8][CH2:7][C:6](=[O:11])[CH3:12])#[N:1]

Participants

5

Reactant 4

HCID 222AmmoniaHCID 887MethanolHCID 977Oxygen2×HCID 114192-Methylcyclohexanone

Product 1

HCID 13081567HCID 13081567, compound

Procedure

A solution of 2 ml of NH3 in 50 ml of methanol is charged into a round bottom flask fitted with a gas inlet tube and a mechanical stirrer. Fitted to the gas inlet tube was an oxygen buret graduated in ml and containing oxygen gas. To this solution was added with stirring 0.015 g of CuCl2.H2O and 1.1 g of 2-methyl cyclohexanone. Stirring was continued until all solids had dissolved. A steady stream of oxygen was bubbled into the solution for approximately 20 hours, while the solution was stirred at room temperature. Total oxygen uptake was 190 ml. The methanol solvent was removed by rotary evaporator and the product extracted in ether. The ether layer was concentrated. IR analyses confirmed the presence of the desired compound and the lack of the oxazoline compound.

Workup

  1. customfitted with a gas inlet tube and a mechanical stirrer
  2. customFitted to the gas inlet tube
  3. additionTo this solution was added
  4. dissolutionhad dissolved
  5. customA steady stream of oxygen was bubbled into the solution for approximately 20 hours, while the solution
  6. stirringwas stirred at room temperature
  7. customThe methanol solvent was removed by rotary evaporator
  8. extractionthe product extracted in ether
  9. concentrationThe ether layer was concentrated

Sources & evidence

ORD record
ord-5859c6bc7fdc4d5b92fa54ccad09ba02
Source dataset
uspto-grants-1983_10
Patent number
US04410705

Reaction notes

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