反应详情

To a stirred mixture of 4-[5-methoxy-1-phenylsulfonyl-1H-indazol-3-yl]-1-piperazinecarbonitrile (9.5 g, 0.0239 mol) in THF (150 ml) under N2 was added, dropwise, lithium aluminum [50 ml (2.1 eq) of a 1M LiAlH4 solution in THF]. After complete addition the reaction was warmed to reflux and stirred for 3 hours. To the cooled reaction was added carefully, H2O (15 ml) to destroy the excess LiAlH4. The mixture was allowed to stand overnight. The reaction mixture was filtered through a coarse sintered glass funnel. The resultant cake was washed well with THF and the THF filtrate was concentrated to afford 6.0 g, of a residue. The residue was triturated with ether and H2O and the resultant solid was collected and dried to afford 4.5 g of 5-methoxy-3-(1-piperazinyl)-1H-indazole, m.p. 163°-169° C.

1. additionwas added
2. additionAfter complete addition the reaction
3. temperaturewas warmed
4. temperatureto reflux
5. customTo the cooled reaction
6. additionwas added carefully
7. customH2O (15 ml) to destroy the excess LiAlH4
8. waitto stand overnight
9. filtrationThe reaction mixture was filtered through a coarse sintered glass funnel
10. washThe resultant cake was washed well with THF
11. concentrationthe THF filtrate was concentrated
12. customto afford 6.0 g
13. customThe residue was triturated with ether and H2O
14. customthe resultant solid was collected
15. customdried