反応 #2386224

反応方程式

p-toluamide

pivaldehyde

benzotriazole

→

title compound

収率 68.1%

N-(1-(1H-1,2,3-Benzotriazol-1-yl)-2,2-dimethylpropyl)-4-methylbenzamide

収率 68.1%

溶媒

toluene

反応条件

後処理

1. 1
   温度The solution was heated
2. 2
   温度at reflux under Dean-Stark conditions for 10 hours
3. 3
   温度further cooled to 5° C
4. 4
   その他The white precipitate which formed
5. 5
   ろ過was collected by filtration
6. 6
   洗浄was washed with 50% diethyl ether/hexanes (100 mL)

実験手順

A suspension of p-toluamide (4.11 g, 30.4 mmol), pivaldehyde (2.62 g, 30.4 mmol), and benzotriazole (3.62 g, 30.4 mmol) in toluene (200 mL) was treated with p-toluenesulfonic acid (286 mg, 1.52 mmol). The solution was heated at reflux under Dean-Stark conditions for 10 hours, cooled gradually to ambient temperature, and further cooled to 5° C. The white precipitate which formed was collected by filtration and was washed with 50% diethyl ether/hexanes (100 mL) to provide 6.67 g of the title compound as a white solid.

出典