反应详情

To 2B (6.30 g, 26.2 mmol) in DMF (52.5 mL) was added HOBT.H2O (4.9 g, 32.0 mmol) and EDC (5.98 g, 31.3 mmol). After stirring 1 h at rt, the reaction was cooled to 0° C. and 25% ammonium hydroxide was added. The reaction was stirred for 1.5 h and was then diluted with ethyl acetate/THF and washed with 1N HCl (2×) and 1 N NaOH (2×). The aqueous layer was back-extracted with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), filtered and concentrated to provide 2C (5 g) as a yellow solid. LC-MS: 240.08 (M+H)+.

1. temperaturethe reaction was cooled to 0° C.
2. stirringThe reaction was stirred for 1.5 h
3. washwashed with 1N HCl (2×) and 1 N NaOH (2×)
4. extractionThe aqueous layer was back-extracted with ethyl acetate
5. washThe combined organic layers were washed with brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated