HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9857126, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,3-Dichloroacetone | HCID 10793 | — |
| Reactant | 4-(Trifluoromethyl)cinnamamide | HCID 5709014 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 9857126 | HCID 9857126 | 63.1% |
Reaction Steps
A mixture of (E)-3-(4-trifluoromethylphenyl)-2-propenamide (17.9 g) and 1,3-dichloroacetone (14.8 g) in toluene (83 ml) was refluxed for 9 hours by use of Dean-Stark apparatus. After cooling, the reaction mixture was combined with water, extracted with ethyl acetate, washed with saturated brine, and dried over magnesium sulfate, then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane:ethyl acetate=6:1 to 5:1) to give the titled compound (15.1 g) as colorless needle crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06984653B2 |
| Source dataset | uspto-grants-2006_01 |
| ORD ID | ord-f5e6a1b5218143e3a243ec9ba534379d |
| Source note | uspto-grants-2006_01 |