HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Bromo-4-chloro-2-fluoro-n-methyl-n-o-tolyl-benzamide → 5-bromo-4-chloro-2-methoxy-N-methyl-N-o-tolyl-benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Bromo-4-chloro-2-fluoro-n-methyl-n-o-tolyl-benzamide | HCID 68602767 | — |
| Reactant | HCID 178501943 | HCID 178501943 | — |
| Product | 5-bromo-4-chloro-2-methoxy-N-methyl-N-o-tolyl-benzamide | HCID 68603605 | — |
Reaction Steps
A mixture of 5-bromo-4-chloro-2-fluoro-N-methyl-N-o-tolyl-benzamide (2.5 g, 7.0 mmol) was heated in MeONa/MeOH (20 mL, 25%) at 55° C. for 12 hrs, then was concentrated and partitioned between DCM and water. The organic layer was then separated, washed with 3N HCl, sat NaHCO3 and brine, dried over MgSO4, and concentrated. Purification by silica gel column chromatography eluting with ethyl acetate in hexanes (1/4) gave 5-bromo-4-chloro-2-methoxy-N-methyl-N-o-tolyl-benzamide (2.75 g). MS: 367.8 (M+H)+; tR=2.51 min (method 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481738B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-852b99300976438c96131f4d445fb822 |
| Source note | uspto-grants-2013_07 |