反応 #992697

反応方程式

aniline

1-naphthoyl chloride

water

ammonium hydroxide

→

solid

収率 82.0%

Naphthalene-1-carboxylic acid phenylamide

収率 82.0%

溶媒

acetonitrile

diethyl ether

反応条件

後処理

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

実験手順

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).

出典