反应详情

温度

115 °C

To a round bottom flask were added N-[4-bromo-2-(trifluoromethyl)phenyl]-2-{[(3S)-1-(cyclopropylcarbonyl)-3-pyrrolidinyl]acetyl}hydrazinecarboxamide (1025 mg, 2.148 mmol) and potassium carbonate (1203 mg, 8.70 mmol). The mixture was suspended in water (100 mL) and refluxed for 16 h at 115° C. Analysis by LCMS indicated consumption of starting material and formation of desired product and by-products related to the starting material. The solution was neutralized to pH=7 with 1N aq HCl and diluted with 150 mL of ethyl acetate. The aqueous phase was extracted with ethyl acetate (3×) and the combined organic layers were washed with brine, dried over sodium sulfate, and concentrated in vacuo. This material was purified by silica gel chromatography (0-20% isopropanol/ethyl acetate), to afford the title product (177 mg, 18%). MS(ES)+ m/e 459.2, 461.2 M+H]+.

1. customconsumption of starting material and formation of desired product and by-products
2. additiondiluted with 150 mL of ethyl acetate
3. extractionThe aqueous phase was extracted with ethyl acetate (3×)
4. washthe combined organic layers were washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThis material was purified by silica gel chromatography (0-20% isopropanol/ethyl acetate)