反应详情

温度

6 °C

16.8 g sodium was added to 500 mL ethanol at 10° C. Then, 48.5 g formamidine hydrochloride was added and the reaction was stirred 15 min at 6° C. 28 g (1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepin-4-yl)-phenyl-methanone was added and the reaction was stirred 17 h at RT and 1 h at 40° C. The mixture was filtered and the solvent was removed. The residue was dissolved in ethyl acetate. The layers were separated and the organic layer was washed with water and evaporated. The residue was crystallized with diethylether to yield 10.7 g of the desired product. Fp: 81-82° C.

1. stirringthe reaction was stirred 17 h at RT and 1 h at 40° C
2. filtrationThe mixture was filtered
3. customthe solvent was removed
4. dissolutionThe residue was dissolved in ethyl acetate
5. customThe layers were separated
6. washthe organic layer was washed with water
7. customevaporated
8. customThe residue was crystallized with diethylether