HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178475125, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 12202377 | HCID 12202377 | — |
| Product | HCID 178475125 | HCID 178475125 | — |
Reaction Steps
To a solution of 1.0 g of 2-acetylamino-3-(o-fluorobenzoyl)thiophene in 10 ml of dimethylformamide is added 0.220 g of 63 % sodium hydride. The mixture is stirred at room temperature for 30 minutes. Then 1.0 g of methyl iodide in 1 ml of dimethylformamide is added thereto. The mixture is stirred at room temperature overnight, then poured into water, and extracted with benzene. The benzene extracts are washed with water, dried over sodium sulfate, and the solvent is removed under reduced pressure. The residual oil is chromatographed on silica gel, using chloroform as an eluent to give crystals, which are recrystallized from ether to give N-methyl-1-acetylamino-3-(o-fluorobenzoyl)thiophene as crystals having a melting point of 94° - 95°C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03957783 |
| Source dataset | uspto-grants-1976_05 |
| ORD ID | ord-19260b73794149ddb99db7a0cb109ad5 |
| Source note | uspto-grants-1976_05 |