반응 #40675

반응 방정식

20a

Ethyl 1-pivaloylpiperidine-4-carboxylate

Lithium aluminum hydride

→

desired product

수율 97.0%

(1-neopentylpiperidin-4-yl)methanol

수율 97.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도to warm to rt
2. 2
   기타The reaction was quenched by slow addition of sodium sulfate hydrated crystals (Na2SO4.10H2O) until there
3. 3
   workup.ADDITIONbubbling on addition
4. 4
   여과The mixture was filtered through Celite®
5. 5
   세척the Celite® washed with diethyl ether
6. 6
   기타The solvent was removed from the filtrate

실험 절차

20a (29.5 g, 122 mmol) was dissolved in 200 mL of tetrahydrofuran and cooled to 0° C. Lithium aluminum hydride (s) (10.6 g, 279 mmol) was added slowly and the reaction was allowed to warm to rt and stirred for 24 h. The reaction was quenched by slow addition of sodium sulfate hydrated crystals (Na2SO4.10H2O) until there was no bubbling on addition followed by 20 mL of water. The mixture was filtered through Celite®, and the Celite® washed with diethyl ether. The solvent was removed from the filtrate to provide 20 g (97%) of the desired product as a white solid. 1H NMR (400 MHz, CDCl3).

출처