反应 #992697

反应方程式

aniline

1-naphthoyl chloride

water

ammonium hydroxide

→

solid

收率 82.0%

Naphthalene-1-carboxylic acid phenylamide

收率 82.0%

溶剂

acetonitrile

diethyl ether

反应条件

后处理

1. 1
   其他To the solution so formed
2. 2
   其他20 min
3. 3
   其他The phases were separated
4. 4
   洗涤the aqueous phase was washed with 100 ml of dichloromethane
5. 5
   其他The organic fractions were collected
6. 6
   干燥dried with magnesium sulfate
7. 7
   过滤filtered
8. 8
   其他the solvent was then removed under reduced pressure

实验过程

4.77 g of 1-naphthoyl chloride (TCI America) was dissolved in 100 ml of anhydrous acetonitrile. To the solution so formed, 2.28 ml of aniline (Sigma-Aldrich) was added in a dropwise fashion over a period of c.a. 20 min. The reaction was then refluxed for 2 h at 82° C. 100 ml of distilled water and 5 ml of concentrated ammonium hydroxide were added along with 100 ml of diethyl ether in a separatory funnel. The phases were separated and the aqueous phase was washed with 100 ml of dichloromethane. The organic fractions were collected and dried with magnesium sulfate, filtered and the solvent was then removed under reduced pressure to yield a white solid 5.07 g (82%; 20.5 mmol).

来源