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温度

0 °C

In a 2 l flask, a mixture of 3-chloropropanol (56.7 g), benzyl bromide (102.6 g) and dry THF (600 ml) is stirred and cooled with ice/salt mixture. Potassium tert-butoxide (70 g) is added in portions (5-10 g), maintaining the internal temperature at about 0° C. After the mixture is stirred for 3 more hours at room temperature, the solvent is evaporated. Addition of 1N HCl (1 l), extraction with ether (1 l), and evaporation of solvent gives crude material (113.6 g), which is distilled under vacuum to give 1-chloro-3-benzyloxypropane (108.4 g) b.p.0.01 60°-80° C.

1. temperaturecooled with ice/salt mixture
2. stirringAfter the mixture is stirred for 3 more hours at room temperature
3. customthe solvent is evaporated
4. additionAddition of 1N HCl (1 l), extraction
5. customwith ether (1 l), and evaporation of solvent
6. customgives crude material (113.6 g), which
7. distillationis distilled under vacuum