Aluminium lithium hydride → HCID 44249494, compound

Participants

Reaction Conditions

Reaction Steps

Lithium aluminium hydride (2.4691 mmol, 0.0938 gram) was taken in a 25 mL two necked round bottom flask provided with a condenser, under nitrogen atmosphere. To this (1H-Indol-5-yl)-(4-methylpiperazin-1-yl)methanone (2.0576 mmol, 0.5 grams) (obtained from step (iii)) dissolved in 5 mL of THF was added and refluxed the mass for a period of 2 hours. After the completion of reaction, the reaction mixture was cooled to 25° C. and quenched by addition of ice-cold water slowly, to decompose the excess of LAH. The resultant precipitate of aluminium hydroxide was removed by filtration over hy-flow. THF was distilled off from this emulsion and the concentrate was diluted with water (20 mL), basified with 20% sodium hydroxide solution to pH: 10 and the mixture was extracted with ethyl acetate (2×20 mL). The combined ethyl acetate extracts were then washed with water (2×20 mL), brine 20 mL and dried over anhydrous sodium sulfate. The volatiles were removed under reduced pressure to obtain thick syrupy mass. This syrupy compound was purified over silica gel column, eluent being ethyl acetate and triethylamine (0.2 to 1.0%).

Provenance & Evidence