HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Thiophosgene → 2-Fluoro-1-isothiocyanato-3-trifluoromethyl-benzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Thiophosgene | HCID 10040 | — |
| Edukt | 3-Amino-2-fluorobenzotrifluoride | HCID 145569 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-Fluoro-1-isothiocyanato-3-trifluoromethyl-benzene | HCID 83402407 | 91% |
Reaktionsschritte
To a two phase solution of 2-fluoro-3-trifluoromethyl-phenylamine (2 g, 11.17 mmole) in dichloromethane (40 ml) and sodium bicarbonate (6.57 g, 78.19 mmole) in water (30 ml) at 0° C. was added dropwise a solution of thiophosgene (1.28 g, 11.17 mmole) in dichloromethane (10 ml). After 2 hrs, the organic layer was separated, washed sequentially with 1M NaHCO3, brine and water. The organic layer was dried over Na2SO4, filtered and concentrated to yield 2.2 g (91%) of product as a viscous liquid. MS (ESI+) m/z 221 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08546374B2 |
| Quelldatensatz | uspto-grants-2013_10 |
| ORD ID | ord-129b74bd61b345f4866dd7506dd37b39 |
| Quellennotiz | uspto-grants-2013_10 |