Ammonium → HCID 23522820, compound

Temperature

2.5 °C

4-piperidinol (2 g, 19.8 mmol) was added to dichloromethane (20 mL), and cooled to an internal temperature of 0-5° C. Then, triethylamine (3.31 mL, 23.7 mmol) was added thereto and stirred for 30 min. Pivaloyl chloride (2.62 g, 21.8 mmol) was dropwise added thereto and heated to room temperature. The reaction mixture was stirred at room temperature for 5 hours. After completion of the reaction, the reaction mixture was mixed with a saturated aqueous solution of ammonium (50 mL) and extracted twice with dichloromethane (50 mL). The organic layer thus obtained was dried over anhydrous magnesium sulfate, and filtered and distilled under reduced pressure to obtain the title compound (3.9 g).

1. temperatureheated to room temperature
2. stirringThe reaction mixture was stirred at room temperature for 5 hours
3. customAfter completion of the reaction
4. extractionextracted twice with dichloromethane (50 mL)
5. customThe organic layer thus obtained
6. dry with materialwas dried over anhydrous magnesium sulfate
7. filtrationfiltered
8. distillationdistilled under reduced pressure

ORD record

ord-63a757ab12af48289f7ae53e71512872

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08853213B2