反应详情

To a suspension of methyl 5-(2-amino-4-benzyloxyphenyl)-6-cyclohexyl-4H-thieno[3,2-b]pyrrole-2-carboxylate (6.30 g, 13.8 mmol), sodium acetate (1.36 g, 16.6 mmol) and acetic acid (0.95 ml, 16.6 mmol) in tetrahydrofuran (100 ml) was added dropwise chloroacetyl chloride (1.32 ml, 16.6 mmol), and the mixture was stirred at room temperature for 2 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with saturated aqueous sodium hydrogen carbonate solution, saturated brine, and dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure. The obtained crude product of methyl 5-[4-benzyloxy-2-(2-chloroacetylamino)phenyl]-6-cyclohexyl-4H-thieno[3,2-b]pyrrole-2-carboxylate (8.22 g) was used for Step 6 without further purification.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed successively with saturated aqueous sodium hydrogen carbonate solution, saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationAfter filtration
5. customthe solvent was evaporated under reduced pressure