反应详情

To a cold solution of (S)-4-benzyl-1-methyl-2-(2-methylsulfanyl-ethyl)-piperazine (0.450 g, 1.7 mmol) in 1,2-dichloroethane (5.0 mL) is added dropwise 1-chloroethyl chloroformate (0.24 mL, 2.2 mmol). After stirring at ambient temperature for 18 hours, the 1,2-dichloroethane is evaporated and 40 mL of methanol is added to the residue. This solution is refluxed for 2 hours. Evaporation of the methanol gives the crude product. Silica gel chromatography, eluting with methylene chloride:2N ammonia/methanol (90:10), gives 0.175 g of the title compound as a light yellow oil; mass spectrum (ion spray): m/z=175 (M+1).

1. customthe 1,2-dichloroethane is evaporated
2. addition40 mL of methanol is added to the residue
3. temperatureThis solution is refluxed for 2 hours
4. customEvaporation of the methanol
5. customgives the crude product
6. washSilica gel chromatography, eluting with methylene chloride