反应详情

2,4-Difluorobenzenesulfonyl chloride (CAS no. 13918-92-8) (4.0 g, 19 mmol) in DCM (10 mL) was added slowly to a solution of 2-(methylamino)ethanol (1.66 mL, 20.7 mmol) in DCM (200 mL) and 10% sodium hydroxide solution (200 mL) at 0° C. The reaction was allowed to warm to room temperature and stirred for 20 hours. The DCM layer was separated and the aqueous re-extracted into DCM (2×50 mL). The combined organic extracts were washed with brine (200 mL), dried (MgSO4), filtered and evaporated under reduced pressure to afford the product (4.7 g, 98%). 1H NMR δ (400 MHz, CDCl3): 1.98 (t, 1H), 2.94 (s, 3H), 3.32 (t, 2H), 3.79 (q, 2H), 6.94-7.03 (m, 2H), 7.89-7.95 (m, 1H).

1. customThe DCM layer was separated
2. extractionthe aqueous re-extracted into DCM (2×50 mL)
3. washThe combined organic extracts were washed with brine (200 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated under reduced pressure