反应详情

1-Amino-cycloheptanecarboxylic acid methyl ester hydrochloride (968 mg, 4.66 mmol), HOBT (105 mg, 0.78 mmol) and 4-acetyl-3-hydroxy-benzoic acid (700 mg, 3.89 mmol) were dissolved in DMF (5 ml). EDIA (3.01 g, 23.3 mmol) and EDC were added and the mixture was stirred at room temperature for 72 h. Then the mixture was partitioned between EA and saturated sodium chloride solution, the aqueous phase was extracted with EA, the combined organic phases were dried over sodium sulfate and evaporated to dryness. The residue was purified by RP HPLC (water/ACN gradient) to yield the title compound.

1. customThen the mixture was partitioned between EA and saturated sodium chloride solution
2. extractionthe aqueous phase was extracted with EA
3. dry with materialthe combined organic phases were dried over sodium sulfate
4. customevaporated to dryness
5. customThe residue was purified by RP HPLC (water/ACN gradient)