反应 #40374
ord-c2a674e1238f4dc8b04cc0d29f019f60
反应方程式
反应条件
后处理
- 1其他rises to 65° C
- 2workup.STIRRINGAfter another 30 minutes' stirring
- 3其他the solid precipitated
- 4过滤filtered
- 5洗涤washed with water
- 6workup.DISSOLUTIONThe crude product is dissolved in ethyl acetate
- 7干燥dried with sodium sulfate
- 8其他evaporated down
- 9其他is precipitated which
- 10过滤is filtered off
- 11其他dried
实验过程
6.2 mL of concentrated sulfuric acid is added dropwise to 15.5 g (87 mmol) of 1-(4-ethylphenyl)-2-methylpropan-2-ol in 4.8 mL (91 mmol) acetonitrile and 15 mL glacial acetic acid within 15 minutes, during which time the temperature rises to 65° C. It is then stirred for one hour, diluted with ice water, and made alkaline with concentrated sodium hydroxide solution. After another 30 minutes' stirring, the solid precipitated is suction filtered and washed with water. The crude product is dissolved in ethyl acetate, dried with sodium sulfate, and evaporated down. The oil remaining is combined with petroleum ether, whereupon a solid is precipitated which is filtered off and dried. Yield: 16.3 g (85%); melting point 90° C.-92° C.