Phosphorus oxychloride → HCID 89524648, compound

Participants

Reaction Steps

To a solution of Example 239A (0.4 g, 2.2 mmol) in pyridine (5 mL) was added POCl3 (2 mL, 22 mmol) at room temperature. and the mixture was refluxed overnight. The reaction mixture was cooled to room temperature and carefully quenched with cold water. The resulting mixture was extracted with EtOAc (2×30 mL). The combined organic phases were washed with brine (10 mL), dried over Na2SO4, filtered and concentrated to obtain a dehydration product 1-(3,6-dihydro-2H-pyran-4-yl)cyclobutanecarbonitrile (0.28 g). This crude material was dissolved in EtOH, followed by the addition of Pd/C. The solution was hydrogenated at room temperature overnight, filtered, and concentrated to obtain the title compound (0.24 g), which was used in the next step without further purification.

Provenance & Evidence