反应 #103483
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08530648B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of tert-butyl 2-oxo-1,9-diazaspiro[5.5]undecane-9-carboxylate [1031927-12-4] (920 mg, 3.26 mmol) in dichloromethane (10 mL) was added TFA (2.53 mL, 32.6 mmol). The solution was stirred for 40 min at rt. After completion of the reaction the mixture was evaporated under reduced pressure and dried under high vacuum (1.90 g, 100%). [1H NMR (400 MHz, DMSO-d6) ♀ ppm 8.59-8.35 (m, 2H), 7.83 (s, 1H), 3.27-3.14 (m, 2H), 3.12-2.98 (m, 2H), 2.17-2.04 (m, 2H), 1.80-1.57 (m, 8H); LCMS RtA=0.20 min, [M+H]+=169.2]. After completion of the reaction the mixture was evaporated under reduced pressure dried under high vacuum (1.90 g, 100%) [1H NMR (400 MHz, DMSO-d6) ♀ ppm 8.59-8.35 (m, 2H), 7.83 (s, 1H), 3.27-3.14 (m, 2H), 3.12-2.98 (m, 2H), 2.17-2.04 (m, 2H), 1.80-1.57 (m, 8H); LCMS RtA=0.20 min, [M+H]+=169.2]
来源 ID: ord-03c164b82c9e4e11948e70ece3956789