反应详情

Toluene (100 ml), ethanol (10.12 g, 219.65 mmol) and 5-chlorovaleric acid (25 g, 183.04 mmol) were added into a 200-ml flask in this order at room temperature and then p-toluenesulfonic acid monohydrate (5.22 g, 27.46 mmol) was charged thereto. The solution was gently heated and subjected to reflux dehydration for 3 to 5 hours. After reflux dehydration, the solution was cooled to around room temperature, added with triethylamine (4.63 g, 45.76 mmol) at room temperature, stirred and then added with silica gel. After stirring for a while, the silica gel was filtered off. After the solvent of the filtrate was removed in vacuum distillation, ethyl 5-chlorovalerate (21.54 g, 72%) was isolated in distillation.

1. temperatureThe solution was gently heated
2. temperatureto reflux dehydration for 3 to 5 hours
3. temperatureAfter reflux dehydration
4. temperaturethe solution was cooled to around room temperature
5. additionadded with silica gel
6. stirringAfter stirring for a while
7. filtrationthe silica gel was filtered off
8. customAfter the solvent of the filtrate was removed in vacuum distillation