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温度

0 °C

DMAP (367 mg, 3.0 mmol) and EDAC (748 mg, 3.9 mmol) were added as solids to a solution of 1,3-dimethylindole-2-carboxylic acid (568 mg, 3.3 mmol) in DMF (5 mL), and the resultant mixture was stirred for 10 minutes under a nitrogen atmosphere at 0° C. A methylene chloride solution of the methyl ester of valine (553 mg, 3.3 mmol, in 5 mL of methylene chloride) was added to the mixture, and the mixture was first stirred for one hour at 0° C. then for 5 hours at room temperature. The reaction mixture was partitioned between ethyl acetate and 5% KHSO4 solution and the aqueous solution was back-extracted with ethyl acetate. The combined ethyl acetate washes were in turn washed with 5% KHSO4 solution saturated sodium bicarbonate solution (2×) and brine, dried over sodium sulfate, and concentrated to give the title product as a yellow syrup (900 mg).

1. waitfor 5 hours at room temperature
2. customThe reaction mixture was partitioned between ethyl acetate and 5% KHSO4 solution
3. extractionthe aqueous solution was back-extracted with ethyl acetate
4. washwashed with 5% KHSO4 solution saturated sodium bicarbonate solution (2×) and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated