反应详情

温度

0 °C

The compound of step 6 (0.139 g, 0.24 mmol), methylamine hydrochloride (0.022 g, 0.32 mmol) and triethylamine (0.17 ml, 0.97 mmol) were dissolved in 2 ml of DMF and cooled to 0° C. TBTU (0.195 g, 0.61 mmol) was added and the solution was stirred at room temperature overnight. Water (8 ml) was then added and the mixture was extracted three times with EA. The combined organic phases were washed with 1 N hydrochloric acid, water, a saturated solution of sodium hydrogencarbonate and brine, dried over sodium sulfate, filtered and evaporated to dryness under reduced pressure. The residue was purified by chromatography on silica gel (DCM/MOH, 100:0, then 96:4) to give 0.065 g of the title compound as a beige solid.

1. extractionthe mixture was extracted three times with EA
2. washThe combined organic phases were washed with 1 N hydrochloric acid, water
3. dry with materiala saturated solution of sodium hydrogencarbonate and brine, dried over sodium sulfate
4. filtrationfiltered
5. customevaporated to dryness under reduced pressure
6. customThe residue was purified by chromatography on silica gel (DCM/MOH, 100:0