Nonseparation assay methods
A technology for analytes and compounds, applied in the field of non-separated determination, which can solve problems such as complex operations
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Embodiment 1
[0130] Embodiment 1. Synthesis of compound 1
[0131]
[0132] Iodocarboxylate NHS esters were synthesized by reacting iodocarboxylic acids with N-hydroxysuccinimide using DCC as a coupling agent. Compounds prepared using methods disclosed in U.S. Patent Application Publication 2005 / 0158815 B .
[0133] Under the protection of argon, dithioester was dissolved in dry DMF (50mL) B (1.808 g, 5.00 mmol) was added NaH (60% in mineral oil, 0.200 g, 5.00 mmol). After 4 h of reaction at room temperature, NHS3-iodopropionate was added A (1.485 g, 5.00 mmol), and the resulting mixture was stirred overnight. DMF was removed in vacuo. use CH 2 Cl 2 / EtOAc (40:1) for column chromatography to obtain 1.770 g of yellow solid compound 1 (Yield 67%). 1 H NMR (400MHz, CDCl 3 ): δ 2.30(s, 3H), 2.74(t, 2H), 2.83(s, 4H), 3.01(t, 2H), 5.31(s, 2H), 6.88(t, 2H), 7.07(m, 2H ), 7.11-7.18 (m, 3H), 7.27 (m, 4H), 7.82 (dd, 1H), 7.89 (dd, 1H) ppm.
Embodiment 2
[0134] Embodiment 2. Synthesis of compound 2
[0135]
[0136] Compounds prepared using methods disclosed in U.S. Patent Application Publication 2005 / 0158815 C . Under the protection of argon, the dithioester C (0.692 g, 1.50 mmol) and NaH (60% in mineral oil, 0.060 g, 1.50 mmol) in anhydrous DMF (20 mL) was stirred at room temperature for 4 hours to give a slightly cloudy solution. Then add 5 mL of NHS 6-iodide hexanoate in DMF A (n=4) (0.661 g, 1.95 mmol). After 16 h, DMF was removed under vacuum. To the residue was added 10 mL of acetone followed by 20 mL of diethyl ether. Decant the supernatant. The precipitate was washed three times in the same procedure. After drying in vacuo, 1.200 g of yellow solid compound was obtained 2 . 1 H NMR (400MHz, CD 3 OD): δ1.15(m, 2H), 1.33-1.47(m, 4H), 2.01(p, 2H), 2.38(t, 2H), 2.67(t, 2H), 2.75(t, 2H), 2.82 (s, 4H), 2.88(t, 2H), 5.32(s, 2H) 5 6.88-6.93 (m, 2H), 7.00 (t, 2H), 7.08-7.28 (m, 7H), 7.83 (d, 1H), 7.92 (d, 1H) p...
Embodiment 3
[0137] Example 3. Synthesis of Compounds 3 and 4
[0138]
[0139] Under the protection of argon, the dithioester C (1.00 g, 2.10 mmol) and NaH (60% in mineral oil, 0.087 g, 2.16 mmol) in anhydrous DMF (20 mL) was stirred at room temperature for 4 hours to give a slightly cloudy solution. Then N-6 iodohexyloxysuccinimide in DMF (5 mL) was added D (0.82g, 2.52mmol). The mixture was stirred overnight, after which time DMF was removed under vacuum. The residue was washed four times with 30 mL of ether to obtain 1.35 g of compound 3.
[0140] compound 3 (0.25g) was dissolved in 5mL of methanol, and 5.0mL of 50% NH 2 OH aqueous solution. After the solution was stirred for 2 days, the solvent was evaporated under vacuum. The residue was washed with 6 x 20 mL of ether to give 0.21 g of compound 4 . 1 H NMR (400MHz, CD 3 OD): δ 1.14(m, 4H), 1.40(m, 4H), 1.94(p, 2H), 2.65-2.71(m, 4H), 2.84(t, 2H), 3.55(t, 2H), 5.31( s, 2H), 6.88 (d, 2H), 6.98 (q, 2H), 7.10 (m, 4H), 7.12...
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