Substituted 1,3-dioxanes and their uses
a technology of 1,3-dioxanes and substituted dioxanes, which is applied in the field of substituted dioxanes containing 1, 3-dioxanes, and can solve problems such as unsatisfactory treatmen
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example 1
General Synthesis of the Compounds
[0122]A genera synthetic scheme for the compounds is shown below:
Esterification of Methoxy-Paraconic Acid
[0123]193 g of methoxy-paraconic acid was dissolved in 600 mL of THF, then CDI (145 g, 899 mmol, 1.1 eq) was added at room temperature over a 10 min period. Absolute ethanol 65 mL (or methanol to make the methyl ester) was added and the reaction mixture was stirred for about 120 min to give 188g of compound 23. (Yield 87%).
Reduction of Racemic Methoxy-Paraconic Acid, Ethyl Ester
[0124]105 g of compound 23 (397 mmol) was dissolved in 700 mL of toluene at 5° C. Then 3 eq. DIBAL-H (1.19 mol, 1.19 L 1M solution) was added, the reaction mixture was stirred for 60 min at room temperature and quenched with methanol. The product compound 24 recrystallized as an oily residue from chloroform / hexanes. Yield: 53 g (237 mmol, 59%).
Wittig Reaction Employing Racemic Lactol-Synthesis of Racemic Diol
[0125]191 g carboxypropyltriphenylphosphonium bromide, anhydrous ...
example 2
Synthesis of Compound 1
[0130]
[0131]Compound 1, shown in Table 1, was synthesized using the method of Example 1. HPLC showed that the compound had greater than 99% purity, and the mass spectra corresponded with the molecular ion and the fragmentation pattern expected for compound 1.
example 3
Synthesis of Compound 4
[0132]
[0133]Compound 4, shown in Table 1, was synthesized using the method of Example 1. HPLC showed that the compound had greater than 99% purity, and the mass spectra corresponded with the molecular ion and the fragmentation pattern expected for compound 4.
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