HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → (3-Trifluoromethylphenyl)thiocarbamic acid O-(4-hydroxymethyl-5-oxo-2,3,4,5-tetrahydrobenzo[b]thiepin-4-ylmethyl)ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-Isothiocyanato-3-(trifluoromethyl)benzene | HCID 137232 | — |
| Edukt | 4,4-bis(hydroxymethyl)-3,4-dihydro-2H-benzo[b]thiepin-5-one | HCID 67073365 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | (3-Trifluoromethylphenyl)thiocarbamic acid O-(4-hydroxymethyl-5-oxo-2,3,4,5-tetrahydrobenzo[b]thiepin-4-ylmethyl)ester | HCID 86633682 | — |
Reaktionsschritte
To a solution of 4,4-bis(hydroxymethyl)-3,4-dihydro-2H-benzo[b]thiepin-5-one (555 mg, 2.33 mmol) in 29 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.35 ml, 2.56 mmol) and 3-(trifluoromethyl)phenyl isothiocyanate (885 μl, 5.82 mmol). The mixture was heated to reflux for 72 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:2 ethyl acetate/hexane). The product was obtained in a yield of 320 mg (31%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07858613B2 |
| Quelldatensatz | uspto-grants-2010_12 |
| ORD ID | ord-a1e199664d9f435fa3086fcdfb25aa66 |
| Quellennotiz | uspto-grants-2010_12 |