N-BOC-3-氮杂环庚酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Compound 69 was prepared according to the procedure described above for the synthesis of compound 37 except that 1-Boc-4-piperidone was replaced with tert-butyl 3-oxoazepane-1-carboxylate and 2,4,5-trifluorobenzoyl-chloride was replaced with 3,4-difluorobenzoylchloride. LCMS (+ESI) m/z=434.2 [M+H]+.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Compound 69 was prepared according to the procedure described above for the synthesis of compound 37 except that 1-Boc-4-piperidone was replaced with tert-butyl 3-oxoazepane-1-carboxylate and 2,4,5-trifluorobenzoyl-chloride was replaced with 3,4-difluorobenzoylchloride. LCMS (+ESI) m/z=434.2 [M+H]+.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Compound 69 was prepared according to the procedure described above for the synthesis of compound 37 except that 1-Boc-4-piperidone was replaced with tert-butyl 3-oxoazepane-1-carboxylate and 2,4,5-trifluorobenzoyl-chloride was replaced with 3,4-difluorobenzoylchloride. LCMS (+ESI) m/z=434.2 [M+H]+.

反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 1-bromo-4-methoxybenzene (0.67 mL, 5.4 mmol) in THF (50 mL) at −78° C. was added n-butyllithium (5 mL, 8 mmol) and the reaction mixture was stirred at −78° C. for 2 h. Then was added tert-butyl 3-oxoazepane-1-carboxylate (1.14 g, 5.4 mmol) at −78° C. and the reaction mixture was warmed to room temperature over 12 h. It was then quenched with saturated NH4Cl at 0° C., and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. The crude product was purified by flash chromatography on silica gel (24 g) using 10% ethyl acetate in hexane to yield tert-butyl 3-hydroxy-3-(4-methoxyphenyl)azepane-1-carboxylate (1.2 g, 57%) as a colorless gum. LCMS: R.T. 1.03 min. LCMS (ES-API), m/z 204 (M-117). the reaction mixture was warmed to room temperature over 12 h It was then quenched with saturated NH4Cl at 0° C. extracted with ethyl acetate The combined organic layers were washed with brine dried over anhydrous sodium sulfate filtered concentrated The crude product was purified by flash chromatography on silica gel (24 g)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Compound 69 was prepared according to the procedure described above for the synthesis of compound 37 except that 1-Boc-4-piperidone was replaced with tert-butyl 3-oxoazepane-1-carboxylate and 2,4,5-trifluorobenzoyl-chloride was replaced with 3,4-difluorobenzoylchloride. LCMS (+ESI) m/z=434.2 [M+H]+.