HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13091948, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Hexamethylphosphoramide | HCID 12679 | — |
| Reactant | Potassium Bromide | HCID 253877 | — |
| Reactant | HCID 13091947 | HCID 13091947 | — |
| Catalyst | 18-Crown-6 | HCID 28557 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 13091948 | HCID 13091948 | 76.6% |
Reaction Steps
A solution of 11 g of 6-methyl-5-heptenyl tosylate in 100 ml of THF were added 10 ml of HMPA, 50 g of potassium bromide and 300 mg of 18-crown-6, and the resulting mixture was refluxed for 5 hours. After cooling, water was added, and the mixture was concentrated, the residue was extracted with pentane 3 times, the combined organic layers were washed with a saturated aqueous solution of sodium hydrogen carbonate water and saturated brine, dried and concentrated to give 8 g of an oily substance. This oily substance was distilled (bp 70° C./5 mm Hg) to yield 5.7 g of a pure bromide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04822804 |
| Source dataset | uspto-grants-1989_04 |
| ORD ID | ord-215c7dc6a5fa4b3cb39fc1bbe6dddc3a |
| Source note | uspto-grants-1989_04 |