반응 #51667

반응 방정식

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

sodium hydroxide

→

2-chloro-6-methanesulfonylmethyl-phenylamine

수율 90.0%

반응 조건

후처리

1. 1
   온도heated in an oil bath
2. 2
   workup.STIRRINGThe homogeneous solution was stirred at this temperature for 90 minutes
3. 3
   온도to cool to room temperature
4. 4
   기타The 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
   여과Filtration
8. 8
   세척washing well with water
9. 9
   기타thorough drying

실험 절차

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%).

출처