HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Formic Acid → tert-Butyl (4-Cyano-2-(methylsulfonyl)phenyl)(phenylsulfonyl)methylcarbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Formic Acid | HCID 284 | — |
| Edukt | tert-Butyl carbamate | HCID 77922 | — |
| Edukt | Benzenesulfinic acid, sodium salt | HCID 2723840 | — |
| Edukt | 4-Formyl-3-(methylsulfonyl)benzonitrile | HCID 58133750 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | tert-Butyl (4-Cyano-2-(methylsulfonyl)phenyl)(phenylsulfonyl)methylcarbamate | HCID 86732345 | — |
Reaktionsschritte
Formic acid (6.2 mL, 164 mmol) is added to a mixture of tert-butyl carbamate (3.05 g, 26.0 mmol), 4-formyl-3-(methylsulfonyl)benzonitrile (5.44 g, 26.0 mmol, preparation according to WO09080199) and sodium benzenesulfinate (4.27 g, 26.0 mmol) in THF (10.0 mL) and water (25.0 mL) and the reaction mixture is stirred at room temperature for 4 days. Water (30 mL) is added and the precipitate is filtered off, washed with water and acetonitrile and dried. Yield: 5.10 g. ESI mass spectrum: [M+H]+=451; Retention time HPLC: 0.59 min (X012_S01).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09440930B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-582eeaa3a7854d5db29ff3a2da6a047e |
| Quellennotiz | uspto-grants-2016_09 |