561314-57-6, 2,8-Diazaspiro[4.5]decan-3-one is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
2,8-Diazaspiro[4.5]decan-3-one (0.12 g, 0.75 mmol) and prop-2-yn-1-yl 3-oxo-9- azabicyclo[3.3.1]nonane-9-carboxylate (0.17 g, 0.75 mmol) were dissolved in DOE (7.5 mL) at rt and titanium isopropoxide (0.66 mL, 2.25 mmol) was added. The reactionmixture was heated to reflux under N2 for 16 h then cooled to rt. STAB (0.80 g, 3.75 mmol) was added, the reaction mixture again heated to reflux for 16 h then cooled to rt. The reaction mixture was quenched with the addition of sat. NaHCO3 sol. (10 mL), diluted with DCM (10 mL) then filtered through a pad of celite. The layers were separated and the aqueous layer was extracted with DCM (4 x 20 mL). The organiclayers were combined and washed with brine, then dried (Mg504). The solvents were removed in vacuo, and the residue was purified by column chromatography (normal phase, [Biotage SNAP cartridge KP-sil 25 g, 40-63 tim, 60 A, 27 mL per mm, gradient 1% to 10% MeOH in DCM]) to give an inseparable mixture of diastereomers This mixture was purified by preparative reversed phase HPLC (Phenomenex Gemini-NX 5im 018 11OA Axia column, 100 x 30 mm, eluting with 15 to 35% MeCN/Solvent B over 14.4 mm at 30 mL/min [where solvent B is 0.2% of (28% NH3/H20) in H20] and collecting fractions by monitoring at 205 nm) to give prop-2-yn-1-yl 3-(3-oxo-2,8- diazaspi ro[4. 5]dec-8-yl)-9-azabicyclo[3. 3.1 ]nonane-9-carboxylate Example 5-2 Isomer 1 (0.02 g, 7%) as a colourless solid and prop-2-yn-1-yl 3-(3-oxo-2,8-diazaspi ro[4. 5]dec-8-yl)-9-azabicyclo[3.3. 1 ]nonane-9-carboxylate Example 5-2 Isomer2(0.03 g, 11%) as a colourless solid.
561314-57-6 2,8-Diazaspiro[4.5]decan-3-one 10559599, apiperidines compound, is more and more widely used in various.
Reference£º
Patent; HEPTARES THERAPEUTICS LIMITED; CONGREVE, Miles Stuart; BROWN, Giles Albert; TEHAN, Benjamin Gerald; PICKWORTH, Mark; CANSFIELD, Julie Elaine; (105 pag.)WO2015/140559; (2015); A1;,
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