Hydrochloric Acid → HCID 178497360, compound

HRID 892338Notes

Reaction equation

HRID 892338 reaction equation
Cl.[F:2][C:3]([F:17])([F:16])[C:4]1[NH:8][C:7]2[CH:9]=[CH:10][C:11]([C:13]([OH:15])=[O:14])=[CH:12][C:6]=2[N:5]=1.[CH3:18]O>>[F:17][C:3]([F:2])([F:16])[C:4]1[NH:8][C:7]2[CH:9]=[CH:10][C:11]([C:13]([O:15][CH3:18])=[O:14])=[CH:12][C:6]=2[N:5]=1

Participants

4

Procedure

Gaseous hydrogen chloride is passed through a solution of 59.7 g (0.241 mol) of 14a in 1,000 ml of methanol for 2 hours, simultaneously boiling under reflux. The methanol is then removed by distillation, and the residue is dissolved in ethyl acetate/water and the pH is adjusted to 7 with 2N solution hydroxide solution. The ethyl acetate phase is separated off, the aqueous phase is extracted twice with ethyl acetate, and the organic phase is washed with sodium chloride solution, dried over Na2SO4 and evaporated.

Workup

  1. temperatureunder reflux
  2. customThe methanol is then removed by distillation
  3. dissolutionthe residue is dissolved in ethyl acetate/water
  4. customThe ethyl acetate phase is separated off
  5. extractionthe aqueous phase is extracted twice with ethyl acetate
  6. washthe organic phase is washed with sodium chloride solution
  7. dry with materialdried over Na2SO4
  8. customevaporated

Sources & evidence

ORD record
ord-225776db8c9e457e8fd9f38867c3ccb9
Source dataset
uspto-grants-1992_06
Patent number
USRE033948

Reaction notes

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