Piperidin-4-ol → HCID 86680290, compound

Participants

Reaction Steps

A mixture of 2.074 g of (±)-(4-chlorophenyl)(2-methyl-2H-pyrazol-3-yl)methanol synthesized in Production Example 174, 942 mg of 4-hydroxypiperidine, 1.949 g of p-toluenesulfonic acid monohydrate, and 100 mL of toluene was heated under reflux for 40 minutes while removing water using a Dean-Stark. To the mixture, 1.949 g of p-toluenesulfonic acid monohydrate was added, and the resulting mixture was further heated under reflux for 4.3 hours while removing water. After the mixture was allowed to cool down, toluene and 22 mL of a 1-N sodium hydroxide aqueous solution were added thereto, and the organic layer was collected by separation. The organic layer was washed with 22 mL of a 1-N sodium hydroxide aqueous solution and with a saturated saline solution in this order. The organic layer was dried over sodium sulfate, and then the solvent was distilled off. Thus, the title compound (2.487 g (87%)) was obtained.

Provenance & Evidence