反应详情

Into a 500 ml four-necked flask equipped with a low temperature condenser, a mechanical stirrer, an additional funnel and a nitrogen inlet tub, are placed 102 ml (0.2 m) of n-butyl lithium. This solution is cooled to -60° with an acetone-dry ice bath. A solution of 45 g (0.2 m) of 2,4-dichlorophenacyl chloride dissolved in 250 ml of dry ether is added dropwise. A constant flow of dry nitrogen is maintained throughout the addition. The rate of addition is adjusted so that the reaction temperature does not exceed -55°. After the addition, the reaction is gradually warmed to -10° and then poured into 500 ml of a mixture of saturated ammonium chloride solution and 10% hydrochloric acid solution. The organic layer is separated and the aqueous layer is further extracted with 100 ml of ether. The combined organic extracts are washed with 10% hydrochloric acid and dried over MgSO4. Solvent is evaporated to give 52 g of a pale yellow oil. This material is further purified by vacuum distillation (110°-120°/0.2 mm) to give 44 g of pure product.

1. customInto a 500 ml four-necked flask equipped with a low temperature condenser, a mechanical stirrer, an additional funnel and a nitrogen inlet tub
2. temperatureThis solution is cooled to -60° with an acetone-dry ice bath
3. additionis added dropwise
4. temperatureA constant flow of dry nitrogen is maintained throughout the addition
5. additionThe rate of addition
6. customdoes not exceed -55°
7. additionAfter the addition
8. temperaturethe reaction is gradually warmed to -10°
9. customThe organic layer is separated
10. extractionthe aqueous layer is further extracted with 100 ml of ether
11. washThe combined organic extracts are washed with 10% hydrochloric acid
12. dry with materialdried over MgSO4
13. customSolvent is evaporated