反应详情

Prepared from ethyl 3-(diethylamino)-5-methoxy-1H-indole-2-carboxylate (Unangst PC, et al., J. Heterocyclic Chem. 1987;24:817) and lithium amide by the procedure described in Example 18, with the exception that dilute acetic acid is substituted for 1.0N HCl during the wash of the ethyl acetate extracts. The crude product is purified by flash chromatography (silica gel, 30% ethyl acetate in dichloromethane elution) to give a foam. The foam is dissolved in ether and treated with gaseous HCl to provide the product salt in 36% yield after recrystallization from acetonitrile; mp 244° C.-dec.

1. washwash of the ethyl acetate
2. customThe crude product is purified by flash chromatography (silica gel, 30% ethyl acetate in dichloromethane elution)
3. customto give a foam
4. customto provide the product salt in 36% yield
5. customafter recrystallization from acetonitrile