反応 #51667

反応方程式

N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide

sodium hydroxide

→

2-chloro-6-methanesulfonylmethyl-phenylamine

収率 90.0%

反応条件

後処理

1. 1
   温度heated in an oil bath
2. 2
   workup.STIRRINGThe homogeneous solution was stirred at this temperature for 90 minutes
3. 3
   温度to cool to room temperature
4. 4
   その他The flask was immersed in an ice bath
5. 5
   workup.ADDITIONthe suspension of the product
6. 6
   workup.STIRRINGwas stirred at this temperature until all was crystalline
7. 7
   ろ過Filtration
8. 8
   洗浄washing well with water
9. 9
   その他thorough drying

実験手順

The crystalline N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide of Step 3 was taken up into 200 ml of 2N solution of sodium hydroxide and stirred and heated in an oil bath heated to 120° C. The homogeneous solution was stirred at this temperature for 90 minutes and slowly allowed to cool to room temperature. The flask was immersed in an ice bath and the suspension of the product was stirred at this temperature until all was crystalline. Filtration, washing well with water and thorough drying afforded 13.96 g of pure crystalline 2-chloro-6-methanesulfonylmethyl-phenylamine (90%).

出典