Ammonia → HCID 178433472, compound

HRID 639692Notes

Reaction equation

HRID 639692 reaction equation
[CH3:1][C:2]1[C:3]([OH:10])=[CH:4][C:5](=O)[O:6][C:7]=1[CH3:8].[NH3:11]>O1CCOCC1>[CH3:1][C:2]1[C:3]([OH:10])=[CH:4][C:5]([OH:6])=[N:11][C:7]=1[CH3:8]

Participants

4

Reactant 2

HCID 222AmmoniaHCID 547129154-Hydroxy-5,6-dimethyl-2H-pyran-2-one

Product 1

HCID 178433472HCID 178433472, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

5,6-Dimethyl-4-hydroxy-2-oxo-2H-pyran (J. Chem. Soc. Perkin Trans 1, 1980, 2272) (10 g, 71 mmol) was dissolved in 66 mL of dioxan and 33 mL of 0.88 NH3 solution and the mixture refluxed for 3 h. The resulting suspension was then allowed to cool to room temperature overnight, filtered and the solid collected and dried in vacuo to provide the title compound as a white crystalline solid (6.5 g). The filtrate was concentrated to approximately 10 mL in vacuo, and a second crop of solid collected by filtration (1.0 g). Both crops were combined and used in the next synthetic step.

Workup

  1. filtrationfiltered
  2. customthe solid collected
  3. customdried in vacuo

Sources & evidence

ORD record
ord-a7684557fdcd425d8c22a9f5da583865
Source dataset
uspto-grants-2010_04
Patent number
US07691877B2

Reaction notes

Loading…