Hydrochloric Acid → HCID 178497360, compound

HRID 1253204Notes

Reaction equation

HRID 1253204 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

Reactant 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 178524166HCID 178524166, compound

Product 1

HCID 178497360HCID 178497360, compound

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-cfb09e3dbc7043fc94434b7892352cda
Source dataset
uspto-grants-1988_05
Patent number
US04748163

Reaction notes

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