HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuryl chloride → HCID 86667468, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | Ethyl 4-(4-chlorophenyl)-3-oxobutanoate | HCID 10847663 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86667468 | HCID 86667468 | 101.7% |
Reaction Steps
To a solution of ethyl 4-(4-chlorophenyl)-3-oxobutanoate (61.0 g, 253 mmol) in DCM (811 mL) in an ice bath was added sulfuryl chloride (34.2 g, 253 mmol) and the resulting solution was allowed to stir at room temperature overnight. The reaction was quenched with saturated sodium bicarbonate solution (200 mL) and the layers separated. The organic layer was washed with brine (100 mL), dried over MgSO4, filtered, and concentrated in vacuo to give 70.8 g of title compound. (100% yield). 1H NMR (400 MHz, CDCl3) δ: 7.33-7.30 (m, 2H), 7.17-7.14 (m, 2H), 4.85 (s, 1H), 4.26 (dq, 1H, J=7.2, 1.2 Hz), 4.02 (d, 1H, J=16.8 Hz), 3.97 (d, J=16.8 Hz, 1H), 1.29 (t, 3H, J=7.2 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796271B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-ac44984159a74d23b09940f3cdb78d0e |
| Source note | uspto-grants-2014_08 |