反应详情

0.54 g of (±)-(1,3,4,9-tetrahydro-beta-carboline-2-yl)-(5-nitro-2,4,6,7-tetramethyldihydrobenzofuran-2-yl)methanone, 1.86 g of zinc, 0.19 g of calcium chloride dehydrate and 30 ml of ethanol were added, followed by heating at reflux overnight. The insoluble matter was filtered through celite and the solvent was distilled off. The reaction solution was mixed with water, extracted with chloroform, washed with saturated saline and dried over anhydrous magnesium sulfate and, after the solvent was distilled off under reduced pressure, the residue was purified by silica gel column chromatography (chloroform:ethyl acetate=50:1) to obtain 0.19 g of the objective product (melting point: 129-133° C.)

1. temperatureby heating
2. temperatureat reflux overnight
3. filtrationThe insoluble matter was filtered through celite
4. distillationthe solvent was distilled off
5. additionThe reaction solution was mixed with water
6. extractionextracted with chloroform
7. washwashed with saturated saline
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationafter the solvent was distilled off under reduced pressure
10. customthe residue was purified by silica gel column chromatography (chloroform:ethyl acetate=50:1)