HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Ethyl-4-(3-fluoro-2-methoxyphenyl)-2-oxo-4-methyl-valerate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 4-(3-Fluoro-2-methoxyphenyl)-4-methyl-2-oxo-pentanoic acid | HCID 17989085 | — |
| Product | Ethyl-4-(3-fluoro-2-methoxyphenyl)-2-oxo-4-methyl-valerate | HCID 17989088 | 90.6% |
Reaction Steps
4.14 g (16.28 mmol) of 4-(3-fluoro-2-methoxyphenyl)-4-methyl-2-oxo-pentanoic acid is dissolved in 97 ml of ethanol, mixed with 1.79 ml of sulfuric acid and refluxed for four hours. The ethanol is drawn off in a rotary evaporator, and the residue is carefully mixed with saturated sodium bicarbonate solution until a pH of 9 is reached. It is extracted twice with 100 ml each of ethyl acetate, and the combined organic extracts are washed with water and then with brine. After the desiccant is dried and filtered off, and after the solvent is spun in, the residue is chromatographed on silica gel (mobile solvent ethyl acetate/hexane). 4.16 g (90.6%) of the desired compound is isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07662821B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-ecbc22b2dfdd46b0bb04000736aeefcf |
| Source note | uspto-grants-2010_02 |