HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
tert-Butyl carbazate → tert-butyl N-(2-methyl-6-nitro-phenyl)-hydrazino-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | tert-Butyl carbazate | HCID 70091 | — |
| Edukt | 2-Fluoro-1-methyl-3-nitrobenzene | HCID 13470957 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | tert-butyl N-(2-methyl-6-nitro-phenyl)-hydrazino-carboxylate | HCID 68969283 | 80% |
Reaktionsschritte
To 250 mg of 2-fluoro-3-methyl-nitrobenzene in 5 mL of DMSO are added 1.065 g of commercial tert-butoxycarbonylhydrazine (5 equivalents). The whole is brought to 100° C. for 10 min under microwave heating. The medium is hydrolyzed and then extracted with ethyl acetate several times. The organic phases are collected, dried on magnesium sulfate, filtered and evaporated under reduced pressure leading to a residue which is purified by chromatography on silica gel (cyclohexane/ethyl acetate: 80/20). 342 mg of product corresponding to the expected product are obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08207373B2 |
| Quelldatensatz | uspto-grants-2012_06 |
| ORD ID | ord-0f4902de3d8b4c33b3b891bd80e88913 |
| Quellennotiz | uspto-grants-2012_06 |