HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dibromoethane → HCID 59216374, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dibromoethane | HCID 7839 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 59216379 | HCID 59216379 | — |
| Reactant | Sodium monohydrate | HCID 71353970 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59216374 | HCID 59216374 | 77.1% |
Reaction Steps
To a suspension of sodium hydrate (0.228 g, 60%, 5.72 mmole) in 15 ml DMF was added nitrile (IV) (1.2 g, 3.9 mmole ) and after stirring for 15 minutes at room temperature 1,2-dibromo-ethane (1.1 g, 5.8 mmole ) in 1.5 ml DMF was added. The resulting mixture was stirred 0.5 hour at room temperature and then more sodium hydrate (0.114 g, 2.86 mmole ) was added and the reaction mixture heated for about 10 minutes at 30-35° C. After cooling the mixture was partitioned between ethylacetate and brine, the organic layer was dried over sodium acetate and concentrated in vacuo. Purification by silica gel column chromatography with 30% -50% ethylacetate in hexane afforded compound (V ) 1 g (77% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08536166B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-1f49391863394a5b9c1ec16952c97f97 |
| Source note | uspto-grants-2013_09 |