反应详情

2-Chloro-1-ethane sulfonyl chloride (51.3 mL, 0.49 mol) in dichloromethane (400 mL) was added dropwise over 2 hours to a solution of tert-octylamine (236.3 mL, 1.47 mol) and triethylamine (68.3 mL, 0.49 mol) in dichloromethane (400 mL) at −18° C. The mixture temperature was maintained between −18° C. and −9° C. during the addition. The mixture was allowed to warm to ambient temperature over 1 hour then washed with 1N HCl (400 mL) and distilled water (2×200 mL). The organic layer was dried with MgSO4, filtered and concentrated in vacuo to give a pale yellow oil. The oil was dried under vacuum at 50° C. to give ethenesulfonic acid (1,1,3,3-tetramethyl-butyl)-amide, 96.0 g (90% yield) as a pale yellow oil.

1. temperatureThe mixture temperature was maintained between −18° C. and −9° C. during the addition
2. washthen washed with 1N HCl (400 mL)
3. distillationdistilled water (2×200 mL)
4. dry with materialThe organic layer was dried with MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customto give a pale yellow oil
8. customThe oil was dried under vacuum at 50° C.