HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 71254939, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 86729692 | HCID 86729692 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71254939 | HCID 71254939 | 64% |
Reaction Steps
To a solution of ethyl 3-(4-fluorophenyl)-3-oxo-2-(2,2,2-trifluoroacetamido)propanoate (271 mg, 0.84 mmol) in anhydrous THF (10 mL) was added Lawesson's reagent (682 mg, 1.69 mmol) in one portion and the resulting solution was refluxed for 22 hrs under nitrogen until no starting material is detected by TLC. The solvent was removed under reduced pressure and the crude material was purified by SiO2 chromatography (80% hexanes/20% DCM to 100% DCM in a linear gradient, product elutes in 50% hexanes/50% DCM) (175 mg, 64% yield). 1HNMR (400 MHz, CDCl3): d 7.50 (m, 2H), 7.15 (t, 2H, J=8.8 Hz), 4.31 (q, 2H, J=6.8 Hz), 1.26 (t, 3H, 7.2 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221805B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-5129d3a244f74fdf8b3fa4d4a9f348f9 |
| Source note | uspto-grants-2015_12 |