反应详情

4-Methoxybenzoic acid (6 g, 39 mmol) was treated with diethylamine (4.45 mL, 43 mmol), TBTU (15 g, 46.8 mmol), disopropylethylamine (10.2 mL, 58.5 mmol) in DMF (40 mL). The mixture was stirred at ambient temperature overnight. The reaction was poured into ice water and the resulting mixture extracted several times with ethyl acetate. The organic layer was washed with a solution of saturated sodium bicarbonate, water and then brine. The organic layer was then dried with sodium sulfate, concentrated and purified by flash chromatography using a gradient of 30 to 70% ethyl acetate in hexanes to obtain a brown oil. Yield=7.8 g. MS (M+H)+ 208.

1. extractionthe resulting mixture extracted several times with ethyl acetate
2. washThe organic layer was washed with a solution of saturated sodium bicarbonate, water
3. dry with materialThe organic layer was then dried with sodium sulfate
4. concentrationconcentrated
5. custompurified by flash chromatography
6. customto obtain a brown oil