Reaktion #2190

Reaktionsgleichung

water

4-chloro-4'-methylsulfonylmethylbenzophenone-hydrazone

chlorosulfonyl isocyanate

ethyl acetate

→

desired product

Ausbeute 81.5%

4-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone

Ausbeute 81.5%

Lösungsmittel

n-hexane

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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%).

Quelle