Sodium Hydroxide → HCID 22928805, compound

Participants

Reaction Steps

D3 (9.6 g, 30 mmol) was suspended in a 2.5M aqueous solution of sodium hydroxide (75 mL). The suspension was refluxed for 15 hours and then allowed to cool. The solution was acidified with 6M HCl (˜40 mL) until no more effervescence was observed (˜pH 2) and then the pH was carefully adjusted to pH 8.5 using 2.5 M aqueous NaOH. The resulting precipitate was collected by filtration, washed with cold water (20 mL) and then dried under vacuum at 40° C. for 15 hours to give the title compound (7.5 g, 100% yield) as a light purple solid (Rf: Baseline (ethyl acetate)). 1H-NMR (300 MHz, DMSO-d6) □ 10.98 (1H, br s), 8.93 (1H, br s), 7.40 (1H, d), 6.93 (1H, dd), 6.79 (1H, dd), 4.51-4.48 (1H, m), 3.35-3.32 (2H, m), 3.02-2.98 (2H, m), 2.55-2.52 (2H, m), 1.78-1.74 (2H, m); m.p.>190° C. (decomp).

Provenance & Evidence