反应详情

To a solution of methyl 3-[1-(4-chlorobenzyl)-3-(t-butylthio)-5-hydroxyindol-2-yl]-2,2-dimethylpropanoate (EP 419,049, Mar. 27, 1991, Example 1, Step C) (350 mg) in acetonitrile (5 mL) were added Cs2CO3 (489 mg) and 80% pure halide (180 mg) from Step 1. The mixture was stirred at room temperature for 18 hr. then the mixture was poured into 25% aq. NH4OAc (50 mL), extracted with ethyl acetate (2×50 mL), washed with brine (50 mL), dried (MgSO4), and evaporated to dryness. Chromatography of the residue on flash silica gel using ethyl acetate:toluene (2:3) as eluant gave the title compound as a white solid; m.p. 152°-155° C.

1. extractionextracted with ethyl acetate (2×50 mL)
2. washwashed with brine (50 mL)
3. dry with materialdried (MgSO4)
4. customevaporated to dryness