反应详情

A mixture of 5-(3-chlorophenoxy)-1-(4-diethylaminophenyl)-2-ethoxycarbonylmethyl-indole-3-carboxylic acid ethyl ester (100 mg, 0.18 mmol, see step (a) above), NaOH (1 M in methanol, 2 mL, 2.0 mmol), NaOH (aq, 1 M, 2 mL, 2.0 mmol) and dioxane (2 mL) was stirred at reflux for 4 h, cooled, acidified to pH 4 with HCl (aq, 1 M) and extracted with EtOAc. The combined extracts were washed with H2O and brine, dried (Na2SO4), concentrated and purified by chromatography. Yield 50 mg (56%), mp 186-191° C.

1. temperatureat reflux for 4 h
2. temperaturecooled
3. extractionextracted with EtOAc
4. washThe combined extracts were washed with H2O and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. custompurified by chromatography