Compounds and methods for the treatment of neurodegenerative diseases
a neurodegenerative disease and compound technology, applied in the field of compound and method for the treatment of neurodegenerative diseases, can solve the problems of brain damage, memory loss, language problems, and interfering with a person's daily life and activities, and achieve the effects of preventing brain damage, preventing brain damage, and preventing brain damag
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example 1
N-Acyloxyalkoxycarbonyl Derivative of DFMO
[0081]
Methylation of DFMO:
[0082]To MeOH (50 mL) is added acetyl chloride (7.14 mL, 10 eq) after stirring for 30 minutes, DFMO (0.01 mole) is added. Stirring is continued for 48 hours. After concentration under vacuum, ethyl acetate (500 mL) is added and the contents neutralized (pH=7.2) with saturated NaHCO3. The organic layer is separated, dried and then concentrated under vacuum to afford the methyl ester of DFMO.
Prodrug 1:
[0083]To a solution of the DFMO methyl ester (1 mmole) in DMF (5 mL) is added triethyl amine (3 mmole) followed by the addition of chloromethyl chloroformate (2.1 mmole). The contents are stirred for 16 hours to afford the intermediate 1A. To the intermediate 1A, is then added sodium acetate (4 mmole). After stirring for another 20 hours, ethyl acetate (100 mL) and brine (100 mL) is added. The organic layer is separated, dried with magnesium sulfate and then concentrated under vacuum to afford Prodrug 1 (Formula (II) whe...
example 2
(Oxodioxolenyl)Methyl Carbamate Prodrug
[0084]
Intermediate 2A
[0085]To 0.05 g of DFMO in acetonitrile (5 mL) is added Hunigs base (400 μL, 2.3 mmole) followed by the addition of di-tert-butyl dicarbonate (250 μL). The contents are stirred overnight (20 hours). After adding DCM (1 mL) and sonicating, additional Di-tert-butyl dicarbonate is added (100 uL) and then after 15 minutes methanol (1 mL) was added. The mixture is stirred for 3 hours after which thin layer chromatography showed one spot. Concentration under vacuum, add ethyl acetate (15 mL) and ice and acidify to pH=4. Extract, dry (MgSO4) and then concentrate under vacuum and purify using isocratic 10% MeOH in DCM to afford Intermediate 2A (100 mg). ESI (M+Na) (405.2)
Intermediate 2B
[0086]To 65 mg (0.00017 mole) of the Intermediate 2A acid in THF / MeOH (9:1) (1 mL) cooled to 0° C. is added TMS diazomethane (170 μL, 2 eq). The mixture is warmed to RT (room temperature) and then stirred for an hour. Acetic acid (200 μL) is added an...
example 3
[0089]
[0090]To 0.1 mmole of the methyl ester of DFMO in DCM (10 mL) cooled to 0° C. is added a 20% solution of phosgene in toluene (0.21 mmole) in the presence of triethylamine (3 eq). After stirring for 24 hours to form the intermediate 3A, 4-(hydroxymethyl)-5-methyl-1,3-dioxol-2-one (0.5 mmole) is then added. Stirring is continued for 24 hours. To the reaction is then added water (5 mL) and then 1 N HCl (5 mL). The organic layer is then separated, dried with sodium sulfate and then concentrated under vacuum to afford Prodrug 3 (Formula (II) where Q1 and Q3 are —C(═O)OCH2-5-methyl-1,3-dioxol-2-one, Q2 and Q are H and Q5 is —CH3).
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