Early senile dementia alpha beta starch spot imaging agent
A technology of radioactive labeling and plaque imaging agent, which is applied in the field of Alzheimer's disease Aβ-amyloid plaque imaging agent, and can solve the problem of unfastened removal
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Embodiment 1
[0027] Embodiment one 11 Synthesis of C-labeled p-Hydroxy Schiff Base Imaging Agent
[0028] Synthesis of precursors:
[0029] Weigh 1.8 g of p-N,N dimethylbenzaldehyde, dissolve it in 30 ml of absolute ethanol, add 1.5 g of p-aminophenol, and reflux for 3 hours. A large amount of pale yellow precipitates were filtered and dried to obtain 2.77 g of pale yellow crystals with a yield of 89%. H NMR (500MHZ, DMSO, δ): 3.0(6H), 6.77(4H), 7.10(2H), 7.71(2H), 8.39(1H), 9.3(1H).
[0030]
[0031] Radiolabeled:
[0032] Weigh 1mg of p-N,N dimethyl, p-hydroxyl Schiff base, dissolve in 0.4ml DMSO, add 10μL of 2N NaOH. into the solution 11 CH 3 1, separated by semi-preparative HPLC, the separation column is a C-18 column, the mobile phase is water: acetonitrile (710: 290 V / V), flow rate 1mL / min, wavelength 280nm. The Rt of the product was 5.5min, and the product peak was collected. Or use a Sep-Pak C-18 column to separate, add 10ml of water to the marker, pass through the C-18 ...
Embodiment 2
[0034] Embodiment two 11 Synthesis of C-labeled m-hydroxyl Schiff base imaging agent
[0035] Synthesis of precursors:
[0036] Weigh 1.8g of p-N,N dimethylbenzaldehyde, dissolve it in 30ml of absolute ethanol, add 1.5g of 3-aminophenol, and reflux for 3 hours. A large amount of pale yellow precipitates were filtered and dried to obtain 2.5 g of pale yellow crystals with a yield of 81%. H NMR (500MHZ, DMSO, δ): 3.0(6H), 5.06(1H), 6.62(2H), 6.7(2H), 6.8(1H), 7.10(1H), 7.44(2H), 8.9(1H).
[0037]
[0038] Radiolabeled:
[0039] Weigh 1mg of p-N,N dimethyl, m-hydroxy Schiff base, dissolve in 0.4ml DMSO, add 10μL of 2N NaOH. into the solution 11 CH 3 1, separated by semi-preparative HPLC, the separation column is a C-18 column, the mobile phase is water: acetonitrile (710: 290 V / V), flow rate 1mL / min, wavelength 280nm. The Rt of the product was 5.5min, and the product peak was collected. Or use a Sep-Pak C-18 column to separate, add 10ml of water to the marker, pass throu...
Embodiment 3
[0041] Embodiment three 11 Synthesis of C-labeled naphthol Schiff base imaging agent
[0042] Synthesis of precursors:
[0043] Weigh 1.8 g of p-N,N dimethylbenzaldehyde, dissolve it in 30 ml of absolute ethanol, add 2.15 g of 5-amino-1-naphthol, and reflux for 3 hours. There was a large amount of brown precipitate, which was filtered and dried to obtain 1.7 g of brown crystals with a yield of 50%. H NMR (500MHZ, DMSO, δ): 3.0(6H), 5.06(1H), 6.6(3H), 7.2(1H), 7.3(2H), 7.4(3H), 8.1(H), 9.1(1H).
[0044]
[0045] Radiolabeled:
[0046] Weigh 1mg of p-N,N dimethyl, naphthol Schiff base, dissolve in 0.4ml DMSO, add 10μL of 2NNaOH. into the solution 11 CH 3 1, separated by semi-preparative HPLC, the separation column is a C-18 column, the mobile phase is water: acetonitrile (710: 290 V / V), flow rate 1mL / min, wavelength 280nm. The Rt of the product was 5.5min, and the product peak was collected. Or use a Sep-Pak C-18 column to separate, add 10ml of water to the marker, pa...
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