反应详情

Intermediate 2 (860 mg, 3 mmol) was dissolved in 15 ml DCM and DIPEA (2.041 ml, 12 mmol). 2-ethyl-3-(3-oxo-morpholin-4-yl)-benzenesulfonyl chloride, Intermediate 6 (911 mg, 3 mmol) in 10 ml DCM was slowly added and the reaction was stirred at RT overnight. After that 300 μl DIPEA were added and the reaction mixture was heated to 40° C. for 30 min. Then the solution was evaporated to dryness, dissolved in ethyl acetate, washed with 1 N HCl, sat. aq. NaHCO3 and brine. The combined organic layers were dried with MgSO4, filtered and evaporated to dryness. The crude product (1.5 g) was used without further purification in the next step.

1. temperaturethe reaction mixture was heated to 40° C. for 30 min
2. customThen the solution was evaporated to dryness
3. dissolutiondissolved in ethyl acetate
4. washwashed with 1 N HCl, sat. aq. NaHCO3 and brine
5. dry with materialThe combined organic layers were dried with MgSO4
6. filtrationfiltered
7. customevaporated to dryness
8. customThe crude product (1.5 g) was used without further purification in the next step