反应详情

Add NaBH4 (0.26 mmol) to a solution of 3-(4-iodophenyl)-4-cyano-5-methylsulfanyl-thiophene-2-carboxylic acid ethyl ester, prepared in example E-3, in 2 mL of EtOH at 0° C. Remove the ice-bath and stir at room temperature. After 30 min, add additional NaBH4 (0.26 mmol) and stir and additional 30 minutes. Remove the solvent in vacuo and extract the residue with 50 mL of 1/9 MeOH/CH2Cl2. Evaporate and chromatograph (hexane:ethyl acetate 3:1) over silica gel to provide the title compound: MS (ES+, m/e): 384 (M+1).

1. customRemove the ice-bath
2. stirringstir and additional 30 minutes
3. customRemove the solvent in vacuo
4. extractionextract the residue with 50 mL of 1/9 MeOH/CH2Cl2
5. customEvaporate