Ethanol → HCID 69517140, compound

HRID 1247550Notes

Reaction equation

HRID 1247550 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-be909abcf589440fb1b0b45fb756a5c8
Source dataset
uspto-grants-2006_10
Patent number
US07129270B2

Reaction notes

Loading…