HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86633685, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,4-Difluoro-1-isothiocyanatobenzene | HCID 518879 | — |
| Reactant | 4,4-Bis(hydroxymethyl)-3,4-dihydro-2H-benzo[b]oxepin-5-one | HCID 67073125 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86633685 | HCID 86633685 | — |
Reaction Steps
To a solution of 4,4-bis(hydroxymethyl)-3,4-dihydro-2H-benzo[b]oxepin-5-one (500 mg, 2.25 mmol) in 28 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.34 ml, 2.48 mmol) and 2,4-difluorophenyl isothiocyanate (734 μl, 5.63 mmol). The mixture was heated to reflux for 72 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:2 tert-butyl methyl ether/cyclohexane). The product was obtained in a yield of 376 mg (43%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07858613B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-b427d66dc2b04007a93ebaba6595347e |
| Source note | uspto-grants-2010_12 |