反应 #2314284

反应方程式

ketone

4-Methoxyphenyl (4-(4-methyl-3-pentenyl)-3-cyclohexenyl)methyl ketone

potassium hydroxide

hydrazine hydrate

→

2-(4-(4-Methyl-3-pentenyl)-3-cyclohexenyl)ethyl-4-methoxybenzene

溶剂

diethylene glycol

反应条件

后处理

1. 1
   温度150° C., all for 30 minutes each, then cooled to room temperature
2. 2
   萃取The reaction mixture is extracted between ethyl ether and water
3. 3
   洗涤the combined organic layers are washed with brine
4. 4
   干燥dried over magnesium sulfate
5. 5
   浓缩The solution is concentrated in vacuo
6. 6
   过滤the product is purified by silica gel filtration

实验过程

To a solution of ketone 2E (R=4-Methyl-3-pentenyl) (10 g) in diethylene glycol (30 mL) is added potassium hydroxide (4.3 g) and hydrazine hydrate (4.5 mL). The solution is sequentially heated to 100° C., 125° C., and 150° C., all for 30 minutes each, then cooled to room temperature. The reaction mixture is extracted between ethyl ether and water, and the combined organic layers are washed with brine and dried over magnesium sulfate. The solution is concentrated in vacuo, and the product is purified by silica gel filtration using 20:1 hexanes:ethyl acetate as an eluent.

来源