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 | US08299077B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-91ad76fd012c4d9a8a94902dfc67e81e |
| Source note | uspto-grants-2012_10 |