反应详情

5-[2-(acetylamino)-4-methyl-1,3-thiazol-5-yl]thiophene-2-sulfonyl chloride, prepared as in Step II of Example 1 (280 mg; 0.84 mmol; 1 eq), is dissolved in DCM (10 ml). N-Methyl piperazine (1.4 g; 16.8 mmol; 20 eq) and DIEA (0.17 ml; 0.98 mmol; 3 eq) are added. After one night reaction, water (1 ml) is added and the solvents evaporated to dryness. The crude product is re-dissolved in DCM and washed with NH4Cl saturated solution, water and dried over MgSO4. After evaporation of the solvents, crude material is precipitated in a mixture of DCM and diethyl ether, affording after filtration, Compound (11) as a white solid (125 mg; 40%).

1. additionis added
2. customthe solvents evaporated to dryness
3. dissolutionThe crude product is re-dissolved in DCM
4. washwashed with NH4Cl saturated solution, water
5. dry with materialdried over MgSO4
6. customAfter evaporation of the solvents, crude material
7. customis precipitated in a mixture of DCM and diethyl ether
8. customaffording
9. filtrationafter filtration, Compound (11) as a white solid (125 mg; 40%)