反应详情

3,5-Dichlorophenylisothiocyanate (5 g, 24.5 mmol) was added by portion to a suspension of the HCl salt of ethyl glycinate (3.4 g, 24.5 mmol) in a mixture of TEA (7.5 ml, 53.9 mmol) and dry DCM (40 ml) while cooling the flask in a water bath. After 60 h at RT, the solution was concentrated to dryness and partitioned between EtOAc and aqueous HCl. The organic layer was washed with water and concentrated. The obtained amorphous solid was washed with Et2O to yield 3-(3,5-dichlorophenyl)-2-thioxoimidazolidin-4-one as an orange solid (5.3 g). 1H NMR (CDCl3): 7.45 (1H, m), 7.25 (2H, m), 4.44 (2H, s).

1. temperaturewhile cooling the flask in a water bath
2. concentrationthe solution was concentrated to dryness
3. custompartitioned between EtOAc and aqueous HCl
4. washThe organic layer was washed with water
5. concentrationconcentrated
6. washThe obtained amorphous solid was washed with Et2O