反应详情

温度

0 °C

Diethylamine (9.1 g, 125 mmol, 1.25 equiv.) was added to a 2%-aqueous NaOH-solution (200 ml) and the resulting mixture was cooled to 0° C. (icebath). At this temperature chloroformic acid hex-3-enyl ester (16.2 g, 100 mmol) in diethyl ether (200 ml) was added over a period of 35 min. After complete addition, the cooling bath was removed and stirring was continued for 1.5 h. The mixture was acidified with 2N aqueous HCl-solution, the phases separated and the organic phase was washed with brine and dried over MgSO4. The crude product was purified via fractionated distillation (74-76° C./0.05 mbar) to yield 18.2 g (92%) of product.

1. additionAfter complete addition
2. customthe cooling bath was removed
3. customthe phases separated
4. washthe organic phase was washed with brine
5. dry with materialdried over MgSO4
6. distillationThe crude product was purified via fractionated distillation (74-76° C./0.05 mbar)