HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 54459581, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Bromomethylcyclopropane | HCID 81503 | — |
| Reactant | HCID 3407084 | HCID 3407084 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 54459581 | HCID 54459581 | 75% |
Reaction Steps
In 100 ml of DMF was dissolved 26.6 g of 2-fluoro-6-trifluoromethylbenzamidoxime and 17.8 g of cyclopropylmethylbromide, and to the solution was added 4.8 g of sodium hydride (60% in oil) at 10° C. over 30 min. The solution was then stirred for 3 hours, and the solution reacted was poured into ice-water and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure and the residue was subjected to silica gel column chromatography to obtain 24.8 g of the objective compound. m.p. 63-64° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05942538 |
| Source dataset | uspto-grants-1999_08 |
| ORD ID | ord-93241904648f42eb892ff94f936cd9a3 |
| Source note | uspto-grants-1999_08 |