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温度

0 °C

A mixture of ethyl 4-oxo-1-piperidinecarboxylate (0.23 mol) and 4-(benzyloxy)-phenyl hydrazine (0.23 mol) in ethanol (400 ml) was stirred and refluxed for 5 hours. The reaction mixture was stirred overnight at room temperature. The solid was filtered off and washed on filter with H2O/2-propanol (200 ml). The precipitate was dissolved in CHCl3 (300 ml), washed with water (2×50 ml), dried, filtered and the solvent was evaporated. The residue was crystallized from CH3CN (300 ml) and cooled to 0° C. The resulting precipitate was filtered off and dried, yielding 51.0 g (63%) of ethyl 1,3,4,5-tetrahydro-8-(phenylmethoxy)-2H-pyrido[4,3-b]indole-2-carboxylate (intermediate 1).

1. temperaturerefluxed for 5 hours
2. stirringThe reaction mixture was stirred overnight at room temperature
3. filtrationThe solid was filtered off
4. washwashed
5. filtrationon filter with H2O/2-propanol (200 ml)
6. dissolutionThe precipitate was dissolved in CHCl3 (300 ml)
7. washwashed with water (2×50 ml)
8. customdried
9. filtrationfiltered
10. customthe solvent was evaporated
11. customThe residue was crystallized from CH3CN (300 ml)
12. filtrationThe resulting precipitate was filtered off
13. customdried