HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → N-(2-Methoxy-5-nitro-phenyl)-N-methyl-propionamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | N-(2-methoxy-5-nitrophenyl)propanamide | HCID 2176144 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-(2-Methoxy-5-nitro-phenyl)-N-methyl-propionamide | HCID 59167877 | 95% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a stirred solution of 11.2 g (50.0 mmol) of (2) in 150 mL of anhydrous THF at 0° C. under the nitrogen, was added 3.0 g (75 mmol) of NaH (60% in oil). The suspension was stirred for 0.5 h at 0° C. and 10 mL (150 mmol) of iodomethane was added at 0° C. After the mixture warmed to room temperature and stirred for 3 h, the reaction was quenched by ice brine and extracted with EtOAc (200 mL). The organic phase was washed with brine, dried (Na2SO4), filtered, evaporated in vacuo and the solid was washed with hexane/EtOAc (9:1) to give pure product N-(2-Methoxy-5-nitro-phenyl)-N-methyl-propionamide (3) as a light yellow solid (11.3 g, 95% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08648104B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-59ff6f68e6c443fbba72cf7dcb37dadf |
| Source note | uspto-grants-2014_02 |