反応 #344780

反応方程式

ammonium chloride

1-nitronaphthalene

potassium hydroxide

→

4-nitro-1-naphthylamine

溶媒

dimethyl sulphoxide

dimethyl sulphoxide

反応条件

後処理

1. 1
   その他being kept at 20° to 25° C
2. 2
   workup.ADDITIONWhen the addition
3. 3
   抽出extracted with methylene chloride
4. 4
   その他After drying
5. 5
   その他removing the solvent

実験手順

3.5 g of 1-nitronaphthalene and 3.3 g of N,N-tetramethylenethiocarbamoylsulphenamide, dissolved in 15 ml of dimethyl sulphoxide, are added dropwise to a vigorously stirred suspension of 6 g of potassium hydroxide in 50 ml of dimethyl sulphoxide, the temperature being kept at 20° to 25° C. When the addition has ended the mixture is stirred for a further 60 minutes, poured into 400 ml of a saturated aqueous ammonium chloride solution and extracted with methylene chloride. After drying and removing the solvent, 4-nitro-1-naphthylamine is obtained with a melting point of 190° to 192° C. The yield is 2.9 g (77%). 1Nitro-2-napthylamine is additionally obtained in a yield of about 2%.

出典