反応 #2190

反応方程式

water

4-chloro-4'-methylsulfonylmethylbenzophenone-hydrazone

chlorosulfonyl isocyanate

ethyl acetate

→

desired product

収率 81.5%

4-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone

収率 81.5%

溶媒

n-hexane

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was further stirred for 16 hours at room temperature
2. 2
   その他The reaction mixture was subjected to liquid separation
3. 3
   洗浄the ethyl acetate layer was washed with water
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
6. 6
   洗浄The residual solid was washed with a solvent mixture of ethyl acetate

実験手順

4-chloro-4'-methylsulfonylmethylbenzophenone-hydrazone (1.3 g) and chlorosulfonyl isocyanate (0.63 g) were added to ethyl acetate (100 ml), and the mixture was stirred for one hour at room temperature. Then, water (100 ml) was added, and the mixture was further stirred for 16 hours at room temperature. The reaction mixture was subjected to liquid separation, and the ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with a solvent mixture of ethyl acetate:n-hexane=4:1, to obtain the desired product (1.2 g, melting point: 189° to 191° C., yield: 80%).

出典