反应 #806302

反应方程式

2-hydroxy-4-methoxybenzaldehyde

sodium acetate

nitroethane

→

2-hydroxy-4-methoxy-benzonitrile

收率 86.0%

溶剂

acetic acid

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at gentle reflux for 12 h
3. 3
   萃取The product was extracted with ethyl acetate (3×200 mL)
4. 4
   洗涤The organic extracts were washed with sodium bicarbonate solution until the aqueous layer
5. 5
   干燥The organic layers were then dried over anhydrous magnesium sulfate
6. 6
   浓缩concentrated in vacuo

实验过程

A mixture of the 2-hydroxy-4-methoxybenzaldehyde (20 g, 128.8 mmol), sodium acetate (35.05 g, 257.6 mmol) and nitroethane (19 mL, 257.6 mmol) in glacial acetic acid (100 mL) was heated at gentle reflux for 12 h. The reaction mixture was then poured into ˜1000 mL of ice water (1:1 ratio of ice and water). The product was extracted with ethyl acetate (3×200 mL). The organic extracts were washed with sodium bicarbonate solution until the aqueous layer had pH ˜8. The organic layers were then dried over anhydrous magnesium sulfate and concentrated in vacuo to afford 2-hydroxy-4-methoxy-benzonitrile as a yellow oil (16.5 g, 86%). It was used without further purification.

来源