反应详情

温度

70 °C

The crude spiro compound (23) (162.8 g; 0.36 mol) was dissolved in methylamine/EtOH solution (Fluka, 8M; 1154 ml; 9.23 mol). Sodium iodide (2.16 g; 0.014 mol) was added and the solution was stirred at 70° C. under N2-atmosphere for 3 days. After cooling the reaction mixture was diluted with water and EtOAc (500 ml each). The aqueous layer was extracted with EtOAc (3×800 ml). The organic layer was washed with brine (500 ml). After drying on Na2SO4 the solvent was evaporated to yield a yellow oil. This oil was purified by column chromatography (SiO2; CH2Cl2/MeOH 90:10; containing 1% 7N NH3/MeOH) to yield 30 g of (24) with a purity of 93% (according to HPLC/MS) and 85 g of (24) with a purity of 96% (115 g; 0.25 mol; 70%).

1. temperatureAfter cooling the reaction mixture
2. extractionThe aqueous layer was extracted with EtOAc (3×800 ml)
3. washThe organic layer was washed with brine (500 ml)
4. customAfter drying on Na2SO4 the solvent
5. customwas evaporated
6. customto yield a yellow oil
7. customThis oil was purified by column chromatography (SiO2; CH2Cl2/MeOH 90:10; containing 1% 7N NH3/MeOH)