Reaktion #452552

Reaktionsgleichung

4-(2,1,3-benzothiadiazolyl)-N-methylpiperazine

vinyl chloroformate

dichloroethane

→

4-(2,1,3-benzothiadiazolyl)-N-vinyloxycarbonylpiperazine

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 25 ml round-bottomed flask equipped with condenser and nitrogen inlet
2. 2
   TemperaturThe reaction was refluxed 16 hours
3. 3
   Temperaturcooled
4. 4
   Sonstigeevaporated
5. 5
   SonstigeThe residue was chromatographed on silica gel
6. 6
   Sonstigethe product fractions collected

Vorschrift

To a 25 ml round-bottomed flask equipped with condenser and nitrogen inlet were added 620 mg (2.64 mmol) of 4-(2,1,3-benzothiadiazolyl)-N-methylpiperazine, 0.224 ml (2.64 mmol) vinyl chloroformate, and 15 ml dichloroethane. The reaction was refluxed 16 hours, cooled, and evaporated. The residue was chromatographed on silica gel using methylene chloride/ethyl acetate as eluent, and the product fractions collected to give yellow solid 4-(2,1,3-benzothiadiazolyl)-N-vinyloxycarbonylpiperazine, 530 mg (69%). NMR (d, CDCl3): 3.6 (m, 4H), 3.8 (m, 4H). 4.4-5.0 (m, 2H), 6.6-7.6 (m, 4H).

Quelle