反应详情

温度

80 °C

A mixture of methyl 3-(methylsulfonamido)thiophene-2-carboxylate (prepared in an analogous manner as described in Example 8, Scheme 8, Step 1, 500 mg, 2.125 mmol), 4-(2-chloroethyl)morpholine hydrochloride (435 mg, 2.338 mmol) and potassium carbonate (646 mg, 4.68 mmol) in dry DMF (13 ml) was heated at 80° C. for 5 h and stirred at RT for 3 days. The solvent was evaporated, the residue was diluted with EtOAc and washed with H2O and brine; the organic layer was dried over Na2SO4, filtered and evaporated. The crude was purified by flash chromatography on silica gel (DCM/EtOAc=8/2 to 7/3 and then DCM/MeOH=95/5) to afford methyl 3-(N-(2-morpholinoethyl)-methylsulfonamido)thiophene-2-carboxylate (Int. 50) (655 mg, 1.880 mmol, MS/ESI+ 348.9 [MH]+).

1. customprepared in an analogous manner
2. customThe solvent was evaporated
3. additionthe residue was diluted with EtOAc
4. washwashed with H2O and brine
5. dry with materialthe organic layer was dried over Na2SO4
6. filtrationfiltered
7. customevaporated
8. customThe crude was purified by flash chromatography on silica gel (DCM/EtOAc=8/2 to 7/3