Development and application of PDE10A receptor targeted positron drug [18F] P10A-1910
A P10A-1910, drug technology, applied in the field of positron drugs, can solve problems such as instability
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Embodiment 1
[0038] Example 1 Synthesis of Labeled Precursor Pre1
[0039] The synthetic route of the labeled precursor Pre1 can refer to Nucl.Med.Biol.2017, 55, 12-18., as follows:
[0040]
[0041] Starting from the raw material compound 3-hydroxyphthalic anhydride 1 (4.9g, 30mmol), using triethylamine (90mmol) as the base, under the heating condition of 50°C, in 1,4-dioxane (60mL) solvent React overnight with the compound β-alanine tert-butyl ester hydrochloride 2 (33mmol). After the reaction, add water to quench the reaction, extract with ethyl acetate, and spin dry to obtain a white solid 3 with a yield of 33%, which can be directly proceed to the next reaction. The crude hydrogen spectrum of compound 3 is 1 H NMR (400MHz, CDCl 3 )δ: 7.58–7.53(m, 1H), 7.36(d, J=7.2Hz, 1H), 7.15(d, J=8.4Hz, 1H), 3.89(t, J=7.3Hz, 2H), 2.63( t,J=7.3Hz,2H), 1.40(s,9H).
[0042] With acetonitrile (50mL) as the reaction solvent, compound 3 (2.9g, 10mmol) and 2-iodopropane (20mmol) were mixed in Cs ...
Embodiment 2
[0046] Example 2 Synthesis of Labeled Precursor Pre2
[0047]
[0048] Compound 8 (120 mg, 0.2 mmol) was dissolved in TFA (1.0 mL) and CHCl 3 (0.3mL), the oxidizing agent oxone (184mg, 0.3mmol) was added, and the reaction was carried out at room temperature for 1 hour. After the reaction, the solvent in the reaction system was removed under reduced pressure. Dissolve the resulting solid with ethanol (5 mL), add 10% Na 2 CO 3 (0.5mL) dissolved SPIAd (95mg, 0.4mmol) in aqueous solution, and continued with 10% Na 2 CO 3 The aqueous solution adjusted the pH value of the reaction system to 9, and reacted at room temperature for 1 hour. After the reaction was completed, the reaction was quenched by adding water, extracted with dichloromethane, and separated by flash column chromatography to obtain a white solid Pre2 with a yield of 72%. 1 H NMR (400MHz, DMSO) δ: 7.95(t, J=8.6Hz, 3H), 7.70(t, J=7.9Hz, 1H), 7.61(d, J=8.5Hz, 2H), 7.42(d, J =8.6Hz,1H),7.36–7.29(m,3H),4.78(p,J=...
Embodiment 3
[0049] Example 3 Synthesis of Standard Substance Inhibitor P10A-1910
[0050]
[0051] With pyridine (10mL) as the reaction solvent, compound 5 (500mg, 0.8mmol), triphenyl phosphite (1.2mmol) and 2-amino-4-methylbenzoic acid 6 (0.8mmol) were mixed under heating conditions at 100°C. ) was reacted for 4 hours, then cooled to room temperature, under the protection of nitrogen, 4-fluoroiodobenzene 9 (0.88 mmol) was added and reacted at 100°C for 4 hours. After the reaction, it was cooled to room temperature, the solvent pyridine was spun off, and a white solid P10A-1910 was obtained by flash column chromatography with a yield of 48%. 1 H NMR (300MHz, CDCl 3 )δ:8.12(d,J=8.1Hz,1H),7.58(dd,J=8.5,7.3Hz,1H),7.40(s,1H),7.35(dd,J=7.3,0.7Hz,1H), 7.32–7.26(m,3H),7.24–7.17(m,2H),7.17–7.13(m,1H),4.69(hept,J=6.1Hz,1H),4.10–4.02(m,2H),2.78( t,J=7.2Hz,2H),2.47(s,3H),1.39(s,3H),1.37(s,3H).
[0052] Two, positron drug in the present invention [ 18 F] Preparation method of P10A-1910
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