Hydrochloric Acid → HCID 14498218, compound

HRID 2108247Notes

Reaction equation

HRID 2108247 reaction equation
C([O:3][C:4]([C:6]1[N:7]([CH:25]([CH3:27])[CH3:26])[CH:8]=[C:9]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)[C:10]=1[C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=1)=[O:5])C.Cl>C(O)C.[OH-].[Na+]>[F:17][C:14]1[CH:13]=[CH:12][C:11]([C:10]2[C:9]([C:18]3[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=3)=[CH:8][N:7]([CH:25]([CH3:27])[CH3:26])[C:6]=2[C:4]([OH:5])=[O:3])=[CH:16][CH:15]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 14498217HCID 14498217, compound

Product 1

HCID 14498218HCID 14498218, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 14798Sodium HydroxideSolvent

Procedure

6.8 g (18.4 mol) of the compound from Example 3 are heated to reflux for 18 hours in 30 ml of ethanol and 3.4 ml of 6N sodium hydroxide solution. The mixture is then acidified using 1N hydrochloric acid and the deposited precipitate is filtered off with suction. The precipitate is dissolved again in ethyl acetate, extracted using 1N hydrochloric acid and saturated sodium chloride solution, dried over sodium sulphate and concentrated to dryness. Recrystallization from ether/petroleum ether yields 4.35 g (69% of theory) of colorless crystals of melting point 212° C.

Workup

  1. filtrationthe deposited precipitate is filtered off with suction
  2. dissolutionThe precipitate is dissolved again in ethyl acetate
  3. extractionextracted
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated to dryness
  6. customRecrystallization from ether/petroleum ether
  7. customyields 4.35 g (69% of theory) of colorless crystals of melting point 212° C.

Sources & evidence

ORD record
ord-b3be8b8a1e124758a13c3c32c55cce09
Source dataset
uspto-grants-1990_06
Patent number
US04937255

Reaction notes

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