HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2(3H)-Benzoxazolone → 3-(3-methyl-3-nitro-butyl)-3H-benzoxazol-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2(3H)-Benzoxazolone | HCID 6043 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 1-Iodo-4-methyl-4-nitro-pentane | HCID 9943063 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 3-(3-methyl-3-nitro-butyl)-3H-benzoxazol-2-one | HCID 57435840 | 132% |
Reaktionsschritte
1.70 g (42.5 mmol) sodium hydride (60%) are added batchwise to a solution of 4.50 g (33.3 mmol) benzoxazol-2-one in 50 mL DMF, while the temperature is kept below 0° C. by cooling. After one hour's stirring a solution of 9.61 g (37.4 mmol) 1-iodo-4-methyl-4-nitro-pentane in 20 mL DMF is added dropwise so that the temperature does not exceed 5° C. The mixture is stirred overnight at ambient temperature and the solvent is distilled off. The residue is taken up in ethyl acetate and washed successively with water and sodium chloride solution, dried with sodium sulphate and evaporated down. 11.0 g oil are obtained. Mass spectroscopy: [M+H]+=265.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07429583B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-2572b530e9004b67923d115b5b647add |
| Quellennotiz | uspto-grants-2008_09 |