Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 3,5-Dimethoxyaniline | HCID 66301 | — |
| Reactant | Ethyl 2-[(2-fluorophenyl)methyl]-3-oxobutanoate | HCID 2758957 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 23500388 | HCID 23500388 | — |
Reaction Steps
Ethyl 2-(2-fluorobenzyl)acetoacetate (2.5 g) in xylene (1 ml) was heated to 150° C. and 3,5-dimethoxyaniline (1.46 g) in xylene (4 ml) was added in small portions during 30 minutes. The reaction mixture was heated at 160° C. for 3 hours and then cooled to room temperature. Methanesulfonic acid (1.7 ml) was added and the mixture was stirred at ambient temperature for 30 minutes. Water was added and the precipitate filtered and dried. The product was triturated with warm ethanol. Yield 0.64 g (21%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06774103B1 |
|---|
| Source dataset | uspto-grants-2004_08 |
|---|
| ORD ID | ord-86bfa7e4d1f9432f9109239beedc87c6 |
|---|
| Source note | uspto-grants-2004_08 |
|---|
