Example 1
1. General Experimental Rules
The chemical reagents used in the present invention are commercially available chemical pure or analytical pure. Melting points are determined using a M. P.50 Melting Point System (the thermometer is uncorrected). 1H-NMR, 13C-NMR spectra are determined by Bruker AV300 (300 MHz) nuclear magnetic resonance spectrometer (TMS is an internal standard, and the mass spectrum is determined by Agilent 1946 A-MSD type mass spectrometer (ESI-MS) and Water Q-Tof mass spectrometer (HRMS). The purity is determined by HPLC. The chromato-graphic column is an Agilent C18 (4.6×150 mm, 3.5 μM) reverse phase column. The mobile phase is methanol:water:trifluoroacetic acid=85:15:0.1.
The solvent is concentrated by an N-1100 rotary evaporator (carried out at 40° C.) manufactured by EYELA Instruments Co., Ltd. Silica gel used for column chromatography is 200-300 mesh silica gel (Qingdao Marine Chemical Factory, division factory), and the eluent is petroleum ether (boiling range of 60-90° C.) and ethyl acetate. The reaction is monitored by a GF254 thin-layer chromatography silica gel plate (Nicotiana deli) of 0.25×0.75 mm specification, and ultraviolet absorption is detected by irradiation with ZF-1 three purpose ultraviolet analyzer (Hangzhou David Science and Education instrument Co., Ltd.).
II. Preparation of Intermediates