HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 53998497, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Butene, 1-bromo-3-methyl- | HCID 70092 | — |
| Reactant | HCID 54036684 | HCID 54036684 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 53998497 | HCID 53998497 | 56.5% |
Reaction Steps
To a suspension of 9.68 g of 60% sodium hydride in 50 ml of anhydrous DMF, there is slowly added a solution of 44.9 g of 3-(3-hydroxy propyl) 1,2-dihydro 2-oxo quinoxaline (obtained in accordance with 1.1) in 450 ml of DMF. The solution is agitated until completion of the liberation of hydrogen, whereupon 36 g of prenyl bromide are added. The resultant solution is agitated overnight at room temperature and then evaporated to dryness under reduced pressure. The brown residue is treated with 150 ml of water and 400 ml of methylene chloride. After evaporation under vacuum, a beige solid is obtained which is recrystallized from 200 ml of toluene. In this way there are isolated 33.8 g of compound 1 in the form of pale yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05198441 |
| Source dataset | uspto-grants-1993_03 |
| ORD ID | ord-105604e94a164ad0882bc0d24f5bc49a |
| Source note | uspto-grants-1993_03 |