HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → HCID 25184799, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 4-[(4-Chlorophenyl)sulfanyl]-6-ethyl-5-fluoropyrimidine | HCID 67542493 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | HCID 25184799 | HCID 25184799 | 89% |
Reaction Steps
131 g of 4-(4-chloro-phenylsulfanyl)-6-ethyl-5-fluoropyrimidine, 103.8 g of N-bromosuccinimide and 7.98 g of azobisisobutyronitrile were dissolved in 850 ml of dichloroethane. The resulting mixture was refluxed for 2 hours, cooled to room temperature, and washed successively with 800 ml of water, 50 g of sodium metabisulfite in 950 ml of water and 500 ml of brine. The resulting solution was concentrated under a reduced pressure and crystallized at 5° C. in 391 ml of isopropanol to obtain the white compound, and the compound was washed with 50 ml of isopropanol at 5° C. to obtain the white title compound (150.7 g, yield: 89%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08263769B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-70aee4bdaa6f4061a20b5013995537d6 |
| Source note | uspto-grants-2012_09 |