HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 54724196, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diketene | HCID 12661 | — |
| Reactant | Chlorophenyl isocyanate | HCID 76833 | — |
| Product | HCID 54724196 | HCID 54724196 | — |
Reaction Steps
A mixture of 2-chlorophenylisocyanate (3.0 g, 19.53 mmol), and diketene (3.3 g, 39.28 mmol) in toluene (10.0 mL) containing triethylamine (0.05 mL) was heated to reflux for 6 h, under an atmosphere of argon. Toluene was distilled in vacuo and the resulting residue was purified by silica gel flash chromatography using 25% EtOAc in hexanes as the eluent to afford the title compound (0.85 g, see ref: Heterocycles 27 (9), 2063, 1988.) as a pale yellow solid: 1H-NMR (CD3OD) δ: 7.63 (m, 1H), 7.52 (m, 2H), 7.4 (m, 1H), 6.14 (s, 1H), 2.58 (s, 3H), and 1.95 (s, 3H); ES-MS m/z=278 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07629363B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-5df68a6357534159a9dad47229749ed1 |
| Source note | uspto-grants-2009_12 |