Ethanol → HCID 69517140, compound

HRID 1836172Notes

Reaction equation

HRID 1836172 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([C:8]([CH3:16])([CH3:15])[CH2:9][C:10](=[O:14])[C:11]([OH:13])=[O:12])[CH:5]=[CH:6][CH:7]=1.S(=O)(=O)(O)O.[CH2:22](O)[CH3:23]>>[CH2:22]([O:12][C:11](=[O:13])[C:10](=[O:14])[CH2:9][C:8]([C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=1)([CH3:16])[CH3:15])[CH3:23]

Participants

4

Reactant 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 21908322HCID 21908322, compound

Product 1

HCID 69517140HCID 69517140, compound

Procedure

5.6 g of 4-(3-fluorophenyl)-4-methyl-2-oxovaleric acid and 0.197 ml of sulfuric acid in 150 ml of ethanol are refluxed for 3 hours. The solvent is distilled off. The residue is taken up in ethyl acetate, washed with saturated sodium bicarbonate solution, dried (Na2SO4) and concentrated by evaporation. After bulb tube distillation, 5.6 g of 4-(3-fluorophenyl)-4-methyl-2-oxovaleric acid-ethyl ester with a boiling point of 130° C./0.04 hPA is obtained.

Workup

  1. distillationThe solvent is distilled off
  2. washwashed with saturated sodium bicarbonate solution
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated by evaporation
  5. distillationAfter bulb tube distillation, 5.6 g of 4-(3-fluorophenyl)-4-methyl-2-oxovaleric acid-ethyl ester with a boiling point of 130° C./0.04 hPA
  6. customis obtained

Sources & evidence

ORD record
ord-946e40bb618f4e0db6bbb52bc50b0450
Source dataset
uspto-grants-2004_08
Patent number
US06777409B2

Reaction notes

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