HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 86658341, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 86658340 | HCID 86658340 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86658341 | HCID 86658341 | 38% |
Reaction Steps
To a solution of N-[3,5-bis(trifluoromethyl)phenyl]-3-chloropropanesulfonamide (7.10) obtained in Reference Example 37 in N,N-dimethylformamide (100 mL) was added sodium hydride (60% in oil, 0.84 g), and the mixture was stirred at room temperature for 3 hr. To the reaction mixture was added saturated ammonium chloride and the solution was partitioned between ethyl acetate and water. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate 90:10-40:60) to give the title compound (2.44 g, yield 38%) as a pale-brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338622B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-a32995d082f34b7bb8f680373d85a495 |
| Source note | uspto-grants-2012_12 |