反应详情

温度

0 °C

In the same way as described in for Compound 154, step 2 using 4-(6-nitro-pyridin-3-yl)-morpholine (2.39 g, 11.43 mmol), tin(II) chloride dihydrate (12.9 g, 57.17 mmol) in MeOH (40 mL) and conc. HCl (12.4 mL). The reaction mixture is concentrated in vacuo cooled to 0° C. and dissolved in water. The aqueous solution is basified using conc. NaOH and extracted with ethyl acetate (3×). The organic layers are combined, dried over MgSO4, filtered and concentrated to afford the title compound (1.77 g, 87%) which is used in the next step without further purification.

1. concentrationThe reaction mixture is concentrated in vacuo
2. dissolutiondissolved in water
3. extractionextracted with ethyl acetate (3×)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated