HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Bromobutyronitrile → 3-bromo-4-chloro-N-[2-(3-cyano-propoxy)-phenyl]-N-methyl-benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Bromobutyronitrile | HCID 21412 | — |
| Reactant | 3-bromo-4-chloro-N-(2-hydroxy-phenyl)-N-methyl-benzamide | HCID 68603117 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-bromo-4-chloro-N-[2-(3-cyano-propoxy)-phenyl]-N-methyl-benzamide | HCID 68603154 | 92.7% |
Reaction Steps
CsCO3 (5.17 g, 15.87 mmol) was added to a solution of 4-bromo-butyronitrile (0.63 mL, 6.35 mmol) and 3-bromo-4-chloro-N-(2-hydroxy-phenyl)-N-methyl-benzamide (1.80 g, 5.29 mmol, Step 3B) in DMF (20 mL). The mixture was stirred at room temperature for approximately 16 hrs and was partitioned between ethyl acetate and water. The ethyl acetate layer was separated, washed with water and brine, and was dried over MgSO4. The organic filtrate was evaporated to yield 3-bromo-4-chloro-N-[2-(3-cyano-propoxy)-phenyl]-N-methyl-benzamide as a light yellow solid (2.0 g). MS [M+H]+: 408.9; tR=2.39 min. (method 1)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481738B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-5e4d1df35e2440a5ac48a5f0c223e81e |
| Source note | uspto-grants-2013_07 |