反应详情

温度

60 °C

A 2 L flask equipped with a stir bar was charged with 1,4-dioxane (300 mL), DMF (40 mL), K2CO3 (10 g) and 3-fluoro-4-nitrobenzoic acid (9.7 g). Mono-N-Boc-1,2-diaminoethane (8.6 g) was added to the reaction mixture and stirred for 12 h at 60° C. The reaction mixture was concentrated and the residue was dissolved in CH2Cl2 (400 mL) and H2O (500 mL). The heterogeneous mixture was transferred to a separatory funnel where the aqueous phase was separated and re-extracted with CH2Cl2 (2×100 mL). The organic phases were combined and washed with H2O (5×100 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to provide the title compound as an orange solid (14 g, 84%).

1. customA 2 L flask equipped with a stir bar
2. concentrationThe reaction mixture was concentrated
3. dissolutionthe residue was dissolved in CH2Cl2 (400 mL)
4. customThe heterogeneous mixture was transferred to a separatory funnel
5. customwhere the aqueous phase was separated
6. extractionre-extracted with CH2Cl2 (2×100 mL)
7. washwashed with H2O (5×100 mL)
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure