반응 #2190

반응 방정식

water

4-chloro-4'-methylsulfonylmethylbenzophenone-hydrazone

chlorosulfonyl isocyanate

ethyl acetate

→

desired product

수율 81.5%

4-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone

수율 81.5%

용매

n-hexane

반응 조건

후처리

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

실험 절차

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%).

출처