反应详情

温度

65 °C

To a mixture of the compound obtained in example 1 (200 mg, 0.53 mol), acetamidine HCl (124.5 mg, 1.32 mmol) and sodium methoxide (98.3 mg, 1.85 mmol) in 7 ml of methanol was stirred at 60-70° C. for 18 hrs under nitrogen atmosphere. Once the reaction is complete, the reaction mass was evaporated under vacuum and the residue was diluted with ethyl acetate and water. The organic layer was washed with water followed by brine, dried over sodium sulfate and concentrated under vacuum. The crude product was purified by column chromatography to get 200 mg (40% yields) of the solid product. MP-more than 300° C.

1. customthe reaction mass was evaporated under vacuum
2. additionthe residue was diluted with ethyl acetate and water
3. washThe organic layer was washed with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under vacuum
6. customThe crude product was purified by column chromatography
7. customto get
8. custom200 mg (40% yields) of the solid product
9. customMP-more than 300° C.