HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonamide → N-(3-bromo-5-fluorobenzyl)methanesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonamide | HCID 72879 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | 3-Bromo-5-fluorobenzaldehyde | HCID 21986246 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | N-(3-bromo-5-fluorobenzyl)methanesulfonamide | HCID 47320493 | 99% |
Reaction Steps
Preparation of 3-bromo-5-fluorobenzaldehyde (XLIX) (2.03 g, 10.0 mmol) in DCE (50 mL) was added methanesulfonamide (1.43 g, 15.0 mmol) and TEA (2.79 mL, 20.0 mmol). The solution was stirred for a few minutes before NaBH(OAc)3 (3.00 g, 14.1 mmol) was added. The reaction was stirred at room temperature overnight. The solvent was removed under vacuum and the residue was partitioned between EtOAc and water. The organic layer was separated, dried over MgSO4 and evaporated under vacuum to give N-(3-bromo-5-fluorobenzyl)methanesulfonamide (L) as a clear oil (2.65 g, 9.39 mmol, 99% yield). ESIMS found C8H9BrFNO2S m/z 282 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08883822B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-08a1ef38271e47dbbbd863e323a99727 |
| Source note | uspto-grants-2014_11 |