Hydrazine hydrate (1:1) → HCID 11411236, compound

Participants

Reaction Steps

The compound from Stage 2 above (1.49 g, 1.88 mmol, 1 eq) is refluxed in 50 mL of EtOH in the presence of hydrazine hydrate (0.5 mL, 16.1 mmol, 8.5 eq) for 6 hrs. The cooled medium is filtered, washed with EtOH, and evaporated. The residue is flash chromatographed on SiO2 (gradient elution pure CH2Cl2 up to 80:18:2 CH2Cl2:MeOH:NH4OH). After evaporation of the pure fractions, 1.09 g of a colorless oil is obtained (yield 88%). TLC SiO2 (90:9:1 CH2Cl2:MeOH:NH4OH) Rf=0.34. MS: m/z=660 (M-H+).

Provenance & Evidence