反应详情

A solution (0.05 M) of [5-(4-chlorophenyl)-6-cyclohexyl-2-(methoxycarbonyl)-4H-thieno[3,2-b]pyrrol-4-yl]acetic acid in DMF at RT was treated with morpholine (2 eq.), DIEA (1.5 eq.) and HATU (2.5 eq.). The mixture was stirred at RT for 8 h, then it was diluted with DCM and washed sequentially with aqueous HCl (1 N), aqueous NaHCO3 (saturated solution) and dried. Evaporation of the solvent under reduced pressure gave a residue which was purified by RP-HPLC (Conditions: Waters X-TERRA MS C18, 10 micron, 19×150 mm; flow: 20 mL/min; Gradient: A: H2O+0.05% TFA; B: MeCN+0.05% TFA; 90% A isocratic for 2 min then linear to 10% A in 9 min) to afford the title compound (51%) as a solid.

1. washwashed sequentially with aqueous HCl (1 N), aqueous NaHCO3 (saturated solution)
2. customdried
3. customEvaporation of the solvent under reduced pressure
4. customgave a residue which
5. customwas purified by RP-HPLC (Conditions
6. wait90% A isocratic for 2 min then linear to 10% A in 9 min