Compound for use in enzymatic reaction and mass spectrometry method
A technology for mass analysis and compounds, applied in analytical materials, biological material analysis, material analysis by electromagnetic means, etc., can solve problems such as insufficient, reduced sensitivity, and unfixed conditions for compound quality analysis.
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Embodiment 1
[0091] HV was synthesized according to the following method.
[0092] [chemical 7]
[0093]
[0094] Add compound B (2.0 g, 4.2 mmol), 4-aminophenol (1.15 g, 10.6 mmol, 2.5 equivalents) as compound A, and DMF (N,N-dimethylformaldehyde) as solvent into the flask replaced with nitrogen. Amide) 5mL, cooled to 0°C. DMAP (N,N-dimethyl-4-aminopyridine 115 mg, 1.3 mmol, 0.3 equivalents) and EDC·HCl (1-(3-dimethylaminopropyl)-3-ethylcarbodiethylene Amine hydrochloride, 890 mg, 4.7 mmol, 1.1 equivalents), and DIEA (N,N-diisopropylethylamine, 546 mg, 4.2 mmol, 1.0 equivalents) were added dropwise while keeping the temperature at 0°C. Raise the temperature to 20°C and react for 3 hours. The reaction solution was poured into 150 mL of water, extracted 5 times with 150 mL of ethyl acetate, and the remaining aqueous phase was extracted 6 times with 50 mL of a 10:1 mixture of dichloromethane / methanol. All the obtained organic phases were combined, washed three times with 50 mL of satu...
Embodiment 2
[0097] HVG was synthesized according to the following method.
[0098] [chemical 8]
[0099]
[0100] Dissolve HV (50 mg, 88.5 μmol) and compound C (109 mg, 226 μmol, 3 equivalents) in DMF 2.0 mL, add cesium carbonate (115 mg, 354 μmol, 4 equivalents) at 20° C., and stir at the same temperature for 16 hours. reacted. The reaction mixture was poured into 20 mL of water, and extracted three times with 20 mL of ethyl acetate. The ethyl acetate extracts were combined, washed three times with 20 mL of saturated brine, dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure at 40°C. The residue was purified by separation TLC (a mixed solution of silica gel, dichloromethane and methanol was used as a developing solvent) to obtain 40 mg (yield 38%) of HVA as compound D as a pale yellow oil.
[0101] [chemical 9]
[0102]
[0103] Under nitrogen flow, HVA (40 mg, 44.7 μmol) was added to 1 mol / L sodium methoxide in methanol solution (8.94 μL...
Embodiment 3
[0118] Analysis was performed under the following high performance liquid chromatography and mass analysis conditions using a high performance liquid chromatography mass analyzer LCMS-2010 manufactured by Shimadzu Corporation.
[0119] HPLC conditions
[0120] HPLC system: Shimadzu 30A system, Shimadzu Corporation
[0121] Analytical column: HITACHI Lachrom Ultra C18 (2.0mm×50mm, 2μm, Hitachi High-Tech Co., Ltd. (Hitachi HITECK))
[0122] Mobile phase A: 0.1% formic acid solution
[0123] Mobile Phase B: Acetonitrile
[0124] Needle cleaning solution: Acetonitrile
[0125] Gradient separation of mobile phase A and mobile phase B was performed according to the time program.
[0126] Time program: Gradient (performed according to the following volume ratios)
[0127] [Table 1]
[0128] time (minutes)
Mobile phase A(%)
Mobile phase B(%)
0.00
80
20
3.00
80
20
7.50
40
60
7.51
80
20
10.00
80
20 ...
PUM
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