反应详情

Benzyl chloride (0.2 mole) was dissolved in dry diethyl ether (200 ml) and added dropwise to magnesium turnings (0.22 g atoms). After all the magnesium had reacted, the solution was refluxed for 1 hour and cooled to room temperature. Phenacyl chloride (0.1 mol) in dry diethyl ether (100 ml) was added dropwise over 1 hour at such a rate as to maintain gentle reflux. The solution was then refluxed for 2 hours, and cooled to room temperature; the mixture was poured into ice and the complex decomposed with ammonium chloride solution. The ethereal solution was washed several times with water (2×200 ml), dried (Na2SO4), and the solvent removed in vacuo to give, as a colourless oil, the crude chlorohydrin which was dissolved in dimethyl formamide (80 ml) and a solution of sodium triazole [prepared from sodium (0.1 g atoms) in methanol (40 ml) and 1,2,4-triazole (0.1 mol)] added dropwise at room temperature. After stirring at room temperature for 2 hours, the solution was warmed at 50° for 3 hours. The solvent was removed in vacuo and the residue poured into water to give a crystalline solid which was recrystallized from ethanol/petroleum ether to give the title compound, m.p. 124.5°.

1. temperaturethe solution was refluxed for 1 hour
2. temperatureto maintain gentle reflux
3. temperatureThe solution was then refluxed for 2 hours
4. temperaturecooled to room temperature
5. additionthe mixture was poured into ice
6. washThe ethereal solution was washed several times with water (2×200 ml)
7. dry with materialdried (Na2SO4)
8. customthe solvent removed in vacuo
9. customto give, as a colourless oil
10. temperaturethe solution was warmed at 50° for 3 hours
11. customThe solvent was removed in vacuo
12. additionthe residue poured into water
13. customto give a crystalline solid which
14. customwas recrystallized from ethanol/petroleum ether