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With ammonium hydroxide; hydrogen; In methanol; at 40℃; under 19001.3 Torr; for 8h;Autoclave;
To a solution of A6.2 (228 g, crude) and 145 mL NH4OH in 1.0 L MeOH was added 30 g Raney Ni. The mixture was stirred in an autoclave at 40 oC under hydrogen atmosphere (25 atm) for 8 h. After filtration, the filtrate was concentrated under reduced pressure to get a pale yellow oil, which was purified by reduced pressure distillation to give the title compound (60 g, 54 %) as a colorless oil.1H NMR (500 MHz, DMSO-d6) delta ppm 1.58 (s, 2H), 3.67 (s, 1H), 6.75 (t, 1H), 6.82 (d, 1H), 7.22 (dd, 1H). LC- MS: [MH]+ = 156.1
60 g
With hydrogen; In methanol; at 40℃; under 19001.3 Torr; for 8h;Autoclave;
To a solution of A3.2 (228 g, crude) and 145 mL NH4OH in1 .0 L MeOH was added 30 g Raney Ni. The mixture was stirred in an autoclave at 40 Cunder hydrogen atmosphere (25 atm) for 8 h. After filtration, the filtrate was concentrated under reduced pressure to get a pale yellow oil, which was purified by reduced pressure distillation to give the title compound (60 g, 54 %) as a colorless oil. 1H NMR (500 MHz, DMSO-d6) O ppm 1.58 (5, 2H), 3.67 (5, 1H), 6.75 (t, 1H), 6.82 (d, 1H), 7.22 (dd, 1H). LC10 MS: [MH] 156.1.
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