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 | 93.9% |
Reaction Steps
To a solution of 3-bromo-5-fluorobenzaldehyde (LXXIX) (2.03 g, 10.01 mmol) in DCE (50 mL) was added methanesulfonamide (1.43 g, 15.01 mmol) and TEA (2.79 mL, 20.02 mmol). NaBH(OAc)3 (3.00 g, 14.13 mmol) was added and stirred at room temperature overnight. The solvent was removed under vacuum and the residue was partitioned between EtOAc and water. The organic layer separated and washed with water, brine, dried over MgSO4 and evaporated under vacuum to produce N-(3-bromo-5-fluorobenzyl)methanesulfonamide (LXXX) as a colorless oil (2.653 g, 9.40 mmol, 93.9% yield). ESIMS found C8H9BrFNO2S m/z 282.0 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673936B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-3ce4fe8a685b46c08a771897e51ec482 |
| Source note | uspto-grants-2014_03 |