Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 41365-75-7, name is 1-Amino-3,3-diethoxypropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H17NO2
General procedure: 3.2. Reaction of Wang Resin 1 with Trichloroacetonitrile and Fmoc-amino Alcohol (Resin 2)Wang resin 1 (1 mmol/g loading, 1 g) was suspended in 10 mL of anhydrous DCM, then 1.5 mL oftrichloroacetonitrile was added, and the resin was left in a freezer for 30 min. Next, a solution of 100 Lof DBU in 2 mL of anhydrous DCM was added, and the slurry was shaken for 1 h. The resin waswashed with anhydrous DCM (3) and anhydrous THF (3). The solution of Fmoc-amino alcohol(3 mmol) in 10 mL of anhydrous THF was added to the resin, followed by the dropwise addition of63 L of a solution of BF3Et2O, and the slurry was shaken for 30 min. Resin 2 was washed THF (3),MeOH (3), and DCM (5). A sample of the resin was washed with MeOH (3) and dried, and10 mg was cleaved with 50% TFA for 30 min, and the product quantified (Fmoc absorbance at 300 nm).Typical loading was between 0.35-0.50 mmol/g.3.3. Acylation with a-Bromocarboxylic Acids (Resins 3 And 13)Resin 2 (1 g) was washed with DCM and DMF, Fmoc was deprotected with 50% piperidine inDMF for 15 min, and the resin was washed with DMF (3) and DCM (5). Reaction of the resinwith a solution of -bromocarboxylic acid (5 mmol) in 10 mL of DCM was carried out in a syringewith a frit, and DIC (2.5 mmol, 386 L) was added. After 5 min, DIU was filtered, and the solutionwas transferred to the syringe with resin 1 and shaken for 1 h. When bromoacetic acid was used,DIEA (2.5 mmol, 436 L) was also added. Then, the resin was washed with DCM (3)._ 3.4. Reaction with Amino-aldehyde Dialkyl Acetal and N-Derivatization (Resin 4)Resin 3 (1 g) was washed with DMF (3), a solution of amino-aldehyde dialkyl acetal (10 mmol)and DIEA (10 mmol, 1.74 mL) in 10 mL of DMF was added, and the slurry was shaken for 2 h.An analytical sample was taken for analysis, reacted with 0.5 M Fmoc-OSu in DCM for 1 h and cleavedwith 50% TFA for 30 min.Resin from the previous step was split into four 250 mg portions, which were washedwith reaction solvent: DCM for sulfonamides (Ns-Cl, Tos-Cl) (1 mmol) and DMSO for 4-fluoro-3-nitrobenzotrifluoride (1 mmol). Then, 3 mL of the reaction solvent and DIEA (1.8 mmol, 174 L) wasadded, and the slurry was shaken for 2 h (in the case of sulfonamides) or overnight (in the case of4-trifluoromethyl-2-nitroaryl). Resin 4 was washed with the reaction solvent (3) and then DCM (3).A sample for analysis was reacted with 0.5 M Fmoc-OSu in DCM for 1 h and cleaved with 50% TFA for30 min.
The synthetic route of 41365-75-7 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Gimenez-Navarro, Vanesa; Krch?ak, Viktor; Molecules; vol. 23; 5; (2018);,
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