HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 21083994, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 21083995 | HCID 21083995 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21083994 | HCID 21083994 | 38.8% |
Reaction Steps
To a mixture of Lawesson's reagent (26.3 mg, 0.065 mmol) and the compound of Example 127 (50 mg, 0.13 mmol) was added toluene (10 mL) and the reaction heated at 110° for 1 h. A further portion of Lawesson's reagent (52.6 mg, 0.13 mmol) was added and reaction heated for 6.5 h. The reaction was diluted with DCM, washed with water, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography (silica, 5–10% EtOAc in DCM) to give the title compound as a yellow solid (10 mg, 20%). δH (MeOH-d4) 7.67 (1H, m), 7.58–7.46 (7H, m), 7.40 (3H, m), 6.48 (1H, d, J 9.6 Hz). LCMS (ES+) RT 3.41 minutes, 397 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176215B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-bb5af583b75a44ac9f9000797a902310 |
| Source note | uspto-grants-2007_02 |