HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl iodide → benzyl N-(4-iodophenyl)-N-methylcarbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | N-Cbz-4-iodoaniline | HCID 1245679 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | benzyl N-(4-iodophenyl)-N-methylcarbamate | HCID 18404743 | 96,2% |
Reaktionsschritte
A stirred solution of N-benzyloxycarbonyl-4-iodoaniline (11.5 g, Reference Example 27) in dimethylformamide (70 ml) was treated portionwise with sodium hydride (⅙ g of a 60% dispersion in oil), under nitrogen and at room temperature. When effervescence had ceased methyl iodide (6.3 g) was added and the mixture was stirred at room temperature for 2 hours, after which it was partitioned between ethyl acetate and water. The organic phase was separated, then dried over magnesium sulphate and then evaporated to give the title compound (11.5 g) as a pink oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06479519B1 |
| Quelldatensatz | uspto-grants-2002_11 |
| ORD ID | ord-da2c498bf9dc44d797f26ef8ea60d3f8 |
| Quellennotiz | uspto-grants-2002_11 |