Piperidine → HCID 12109354, compound

Into a device similar to that used in Example 7 were charged 1.05 g (5.0 mmol) of tetrahydropyranyl-4-methanesulfonate synthesized in Example 5 and having a purity of 86% and 1.28 g (15.0 mmol) of piperidine, and the mixture was reacted at 100° C. for 4 hours. After completion of the reaction, 1.0 ml of 8 mol/l aqueous sodium hydroxide solution and 2.0 ml of water were added to the resulting reaction mixture to make the mixture basic (pH=11), the resulting mixture was extracted twice with each 30 ml of chloroform and the extract was dried over anhydrous magnesium sulfate. After filtration, the extract was concentrated under reduced pressure to obtain 0.74 g (yield: 72%) of 4-piperidinotetrahydropyrane having a purity of 82% (areal percentage according to gas chromatography) as a yellowish liquid.

1. customthe mixture was reacted at 100° C. for 4 hours
2. additionwere added to the resulting reaction mixture
3. extractionthe resulting mixture was extracted twice with each 30 ml of chloroform
4. dry with materialthe extract was dried over anhydrous magnesium sulfate
5. filtrationAfter filtration
6. concentrationthe extract was concentrated under reduced pressure

ORD record

ord-9b05e1e8b847439bbc36c902e4fbdcf0

Source dataset

uspto-grants-2003_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06653489B2