反应详情

2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (1.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated and partitioned between EtOAc and H2O. The organic layer was separated and washed sequentially with dilute HCl and saturated brine, then dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88 NH3 90/10/1, v/v). MS m/z 136 (MH+).

1. temperaturethe reaction was warmed
2. temperaturemaintained
3. temperatureat reflux for 2 h
4. temperatureOn cooling
5. customthe reaction mixture was evaporated
6. custompartitioned between EtOAc and H2O
7. customThe organic layer was separated
8. washwashed sequentially with dilute HCl and saturated brine
9. dry with materialdried over Na2SO4
10. customevaporated
11. temperatureheated
12. temperatureat reflux for 2 h
13. customafter which time the mixture was evaporated
14. customtriturated with EtOAc