반응 #801017

반응 방정식

linoleyl methane sulfonate

lithium bromide

→

yellowish oil

수율 117.2%

Linoleyl Bromide

수율 117.2%

용매

acetone

반응 조건

후처리

1. 1
   여과The resulting suspension was filtered
2. 2
   세척the solid washed with acetone
3. 3
   세척The filtrate and wash
4. 4
   기타solvent evaporated
5. 5
   workup.ADDITIONThe resulting residual was treated with water (300 mL)
6. 6
   추출The aqueous phase was extracted with ether (3×150 mL)
7. 7
   세척The combined ether phase was washed with water (200 mL), brine (200 mL)
8. 8
   건조dried over anhydrous Na2SO4
9. 9
   기타The solvent was evaporated

실험 절차

A mixture of linoleyl methane sulfonate (26.6 g, 77.2 mmol) and lithium bromide (30.5 g, 350 mmol) in acetone (350 mL) was stirred under nitrogen for two days. The resulting suspension was filtered and the solid washed with acetone. The filtrate and wash were combined and solvent evaporated. The resulting residual was treated with water (300 mL). The aqueous phase was extracted with ether (3×150 mL). The combined ether phase was washed with water (200 mL), brine (200 mL) and dried over anhydrous Na2SO4. The solvent was evaporated to afford 29.8 g of yellowish oil. The crude product was purified by column chromatography on silica gel (230-400 mesh, 700 mL) eluted with hexanes. This gave 20.8 g (82%) of linoleyl bromide (II).

출처