反应详情

5,6-Bis(acetoxy)-1-aminomethyl-3-phenylnaphthalene hydrochloride (130 mg, 0.34 mmol) from Step 3 was dissolved in 10 mL of methanol saturated with hydrogen chloride. The resultant solution was stirred at ambient temperature for 3 h and then concentrated in vacuo. The solid residue was dissolved in a minimal amount of ethanol. The ethanol solution was added slowly to 30 mL of dry diethyl ether and the precipitate was collected by filtration. The solid was dried at 60° C. in vacuo to give 77 mg (76% yield) of the title compound as a white solid, m.p. 205°-212° C. (dec); DCI MS M/Z: 266 (M+H)+, 283 (M+NH4)+ ; 1H NMR (d6 -DMSO) δ: 4.50 (d, 2H), 7.28 (d, 1H), 7.36-7.60 (m, 4H), 7.77 (s, 1H), 7.83 (d, 2H), 8.35 (s, 1H), 8.49 (br s, 3H), 9.22 (br s, 1H), 9.60 (br s, 1H).

1. concentrationconcentrated in vacuo
2. dissolutionThe solid residue was dissolved in a minimal amount of ethanol
3. additionThe ethanol solution was added slowly to 30 mL of dry diethyl ether
4. filtrationthe precipitate was collected by filtration
5. customThe solid was dried at 60° C. in vacuo