反应详情

温度

100 °C

To a solution of compound 1b (2.4 g, 13 mmol) in DMF (20 mL), Na2HPO4 (4.7 g, 33 mmol) was added followed by tert-butyl 3-(2-bromoacetyl)azetidine-1-carboxylate (6.0, 21 mmol). The resulting mixture was stirred at 100° C. for 3 h. The reaction mixture was allowed to cool to rt and water (50 mL) was added. The aqueous layer was extracted with EtOAc (3×25 mL). The combined EtOAc layers were dried over Na2SO4, filtered, and concentrated. The residue obtained was purified by flash column chromatography on silica gel (0:1-1:0 EtOAc/hexanes) to obtain compound 29a. Mass Spectrum (LCMS, ESI pos.): Calcd. for C18H25N5O3: 360.2 (M+H). found: 360.3.

1. temperatureto cool to rt
2. extractionThe aqueous layer was extracted with EtOAc (3×25 mL)
3. dry with materialThe combined EtOAc layers were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue obtained
7. customwas purified by flash column chromatography on silica gel (0:1-1:0 EtOAc/hexanes)