反応 #1328420

反応方程式

methyl 2-chlorosulfonyl-4-chlorobenzoate

→

Methyl 2-mercapto-4-chlorobenzoate

溶媒

hydrochloric acid

—

ice

反応条件

後処理

1. 1
   workup.WAITAfter 2 hours at this temperature
2. 2
   温度the mixture was cooled
3. 3
   workup.WAITto stand at room temperature for 12 hours
4. 4
   抽出extracted with ethyl acetate
5. 5
   その他the combined organic phases were dried
6. 6
   その他the solvent was removed

実験手順

Over a period of 1.5 hours, 243.5 g (3.7 mol) of zinc powder were added a little at a time to a suspension of 205 g (0.75 mol) of methyl 2-chlorosulfonyl-4-chlorobenzoate in 1 l of concentrated hydrochloric acid and 375 g of ice. The mixture was stirred for another 3 hours and slowly heated to 70° C. After 2 hours at this temperature, the mixture was cooled. The reaction mixture was allowed to stand at room temperature for 12 hours and then extracted with ethyl acetate, the combined organic phases were dried and the solvent was removed. This gave 125.4 g (83%) of methyl 2-mercapto-4-chlorobenzoate.

出典