HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanesulfonyl chloride → (S)-3-(tert-butoxycarbonylamino)-4-(4-chlorophenyl)butyl methanesulfonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanesulfonyl chloride | HCID 31297 | — |
| Edukt | (S)-tert-Butyl 1-(4-chlorophenyl)-4-hydroxybutan-2-ylcarbamate | HCID 57950531 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | (S)-3-(tert-butoxycarbonylamino)-4-(4-chlorophenyl)butyl methanesulfonate | HCID 57950570 | 94% |
Reaktionsschritte
To a mixture of (S)-tert-Butyl 1-(4-chlorophenyl)-4-hydroxybutan-2-ylcarbamate (686 mg, 2.3 mmol) and TEA (399 μl, 2.9 mmol) in DCM (10 mL) at −8° C. was added methanesulfonyl chloride (214 μl, 2.7 mmol). The resulting mixture was stirred for 2 hours. After warming to room temperature, the mixture was diluted with DCM and washed with H2O (2×). The combined organic layers were dried over Na2SO4, filtered, and concentrated to give the product as a light yellow solid (815 mg, 94%). LCMS (API-ES) m/z: 400 (M+Na+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07897619B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-212a2d19de924ef1afb40824f29da493 |
| Quellennotiz | uspto-grants-2011_03 |