137052-08-5, 1-(Tetrahydro-2H-pyran-4-yl)ethanone is a Tetrahydropyrans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
A solution of 1-tetrahydro-2H-pyran-4-ylethanone (351 mg; 2.74 mmol), intermediate11(600 mg; 1.83 mmol), Ti(OiPr)4 (870 jiL; 2.92 mmol) in EtOH (3 mL) was stirred for2 hours at 45C. Additional EtOH (18 mL) and NaBH4 (138 mg; 3.65 mmol) were added.The reaction mixture was stirred at room temperature for 5 hours. The reaction mixturewas diluted with DCM and poured onto a 10% aqueous solution of K2C03. The insolublematerial was removed by filtration over celite. The organic layer was separated, washedwith water, dried over MgSO4, filtered and evaporated to dryness. The residue waspurified by chromatography over silica gel (irregular SiOH, 24g; mobile phase : gradientfrom 0% NH4OH, 0% MeOH, 100% DCM to 1% NH4OH, 10% MeOH, 90% DCM).The fractions containing the product were collected and evaporated to dryness yielding487 mg (60%) of compound 145. The enantiomers of compound 145 were separated bychiral SFC (CHIRALPAK AD-H 5.im 250*30mm; mobile phase: 70% C02, 30%mixture of EtOH/iPrOH 50/50 v/v). The fractions containing the products were collectedand evaporated to dryness. The residues were freeze dried from from water/ACN (80/20;10 mL)yielding 171mg (21%) of compound 154 and 178mg (22%) of compound 155.
137052-08-5, The synthetic route of 137052-08-5 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; JANSSEN PHARMACEUTICA NV; ANGIBAUD, Patrick, Rene; PANDE, Vineet; HERKERT, Barbara; KROSKY, Daniel, Jason; QUEROLLE, Olivier, Alexis, Georges; PILATTE, Isabelle, Noelle, Constance; PATRICK, Aaron, Nathaniel; (250 pag.)WO2018/50686; (2018); A1;,
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