HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoyl Peroxide → N-(4-chlorophenyl)-2-[((5-(bromomethyl)-3-chlorothiophen-2-yl)carbonyl)amino]-5-chlorobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoyl Peroxide | HCID 7187 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 3-chloro-N-{4-chloro-2-[(4-chlorophenyl)carbamoyl]phenyl}-5-methylthiophene-2-carboxamide | HCID 18376748 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | N-(4-chlorophenyl)-2-[((5-(bromomethyl)-3-chlorothiophen-2-yl)carbonyl)amino]-5-chlorobenzamide | HCID 18376771 | 75% |
Reaction Steps
To a suspension of N-(4-chlorophenyl)-2-[((5-methyl-3-chlorothiophen-2-yl)carbonyl)amino]-5-chlorobenzamide (2.6 g, 6.0 mmol) in dry benzene (250 mL) were added N-bromosuccinimide (1.2 g, 6.6 mmol) and benzoyl peroxide (0.15 g, 0.6 mmol). The mixture was refluxed while irradiating with a 250 Watt lamp. After 28 hours the reaction was concentrated of all volatiles in vacuo and the resulting solid triturated with benzene. Purification by flash chromatography on silica gel afforded 2.3 g (75% yield) of N-(4-chlorophenyl)-2-[((5-bromomethyl-3-chlorothiophen-2-yl)carbonyl)amino]-5-chlorobenzamide as a white solid; NMR (DMSO-d6) 11.1 (s, 1), 10.7 (s, 1), 8.3 (d, 1), 7.9 (s, 1), 7.7 (d, 2), 7.6 (d, 1), 7.4 (d, 2), 7.3 (s, 1), 4.9 (s, 2) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06140351 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-6a5d609db4a14b8da882832c83aea8d3 |
| Source note | uspto-grants-2000_10 |