反应详情

To a solution of 2-bromoethylsulfonate sodium salt (25.6 g, 125 mmol) and sodium methoxide (8.03 g, 149 mmol) in EtOH (350 mL) at 0° C. was added, dropwise, a solution of 1,2-ethanedithiol (5.00 mL, 59.4 mmol) in EtOH (25 mL). The reaction mixture was allowed to warm to room temperature, and then heated to reflux for 48 hours. Next, the mixture was cooled to room temperature, and then acidified with 2 N HCl to pH 1-2. The resulting suspension was heated to 75° C. and water was slowly added in small portions until a clear solution was obtained. The reaction mixture was then cooled to room temperature, and then to 5° C. The resulting white precipitate was filtered off, washed with cold EtOH and dried, giving 11.9 g (64.6%) of Compound 4 as a white powder. 1H NMR (500 MHz, D2O) δ 3.27 (t, J=9.3, 6.4 Hz, 4H), 3.06-2.99 (m, 4H), 2.98 (s, 4H). 13C NMR (126 MHz, D2O) δ 51.11, 31.09, 25.58.

1. temperatureheated
2. temperatureto reflux for 48 hours
3. temperatureNext, the mixture was cooled to room temperature
4. temperatureThe resulting suspension was heated to 75° C.
5. customwas obtained
6. temperatureThe reaction mixture was then cooled to room temperature
7. customto 5° C
8. filtrationThe resulting white precipitate was filtered off
9. washwashed with cold EtOH
10. customdried