反应详情

To a solution of Intermediate 229A (100 mg, 0.735 mmol) and TEA (0.102 mL, 0.735 mmol) in DCM was added methanesulfonyl chloride (0.059 mL, 0.735 mmol) dropwise at 5° C. and the reaction mixture was stirred for 3 h. The reaction mass was diluted with DCM, washed with water and brine, dried over Na2SO4, filtered and the filtrate evaporated under reduced pressure. The crude product was purified by silica gel chromatography (12 g REDISEP® column, eluting with 30% EtOAc in petroleum ether). Fractions containing the product were combined and evaporated to afford the Intermediate 229B as a yellow oil (100 mg, 63.5%). 1H NMR (400 MHz, DMSO-d6) δ ppm 4.27 (s, 2H), 3.01 (s, 3H), 2.55-2.69 (m, 2H), 2.06-2.37 (m, 2H), 1.15 (s, 3H).

1. washwashed with water and brine
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. customthe filtrate evaporated under reduced pressure
5. customThe crude product was purified by silica gel chromatography (12 g REDISEP® column, eluting with 30% EtOAc in petroleum ether)
6. additionFractions containing the product
7. customevaporated