反应详情

To a mixture of 2 g (10.6 mmol) of 1-carbomethoxy-3,4-dihydronaphthalene, from Step 1 of Example 46, and 2.08 g (10.6 mmol) of 2-(3-nitrophenyl)-1-nitroethane, from Step 2, in 1 mL of acetonitrile was added 0.2 mL of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). The reaction mixture was stirred at ambient temperature for 0.5 h and then diluted with ethyl acetate. The reaction mixture was washed with 2N aqueous hydrochloric acid solution. The organic layer was separated, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give 3.96 g (97% yield) of the title compound as a mixture of diastereomers which was taken on without purification to the next step; MS DCl--NH3M/Z: 402 (M+NH4)+ ; 1H NMR (CDCl3) δ1.52-1.86 (1H, m), 2.1-2.35 (1H, m), 2.42-2.65 (1H, m), 2.78-3.15 (2H, m), 3.2-3.33 (1H, m), 3.38-3.55 (1H, m), 3.78-3.81 (3H, s), 3.91-4.18 (1H, m), 4.68-4.88 (1H, m), 7.12-7.42 (4H, m), 7.48-7.58 (2H, m), 8.01-8.18 (2H, m).

1. washThe reaction mixture was washed with 2N aqueous hydrochloric acid solution
2. customThe organic layer was separated
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo