反应详情

温度

0 °C

First, N-benzyl-pyrrolidine-3-methanol was prepared as follows. Methyl N-benzyl-5-oxo-pyrrolidine-3-carboxylate (11.66 g, 50 mmol) was dissolved in diethyl ether and cooled to 0° C. This solution was added to a 0° C. suspension of lithium aluminum hydride in diethyl ether under nitrogen atmosphere. After addition, the mixture was refluxed for 1 hr, and then cooled with an ice bath. To quench the reaction, sodium sulfate decahydrate was added and the mixture was stirred for 1 hr. After filtration, the filtrate was collected, and concentrated to dryness to give N-Benzyl-pyrrolidine-3-methanol. ESMS (C12H17NO): calcd. 191.13; obsd. 192.2 [M+H]+. Retention time (anal. HPLC: 10-70% MeCN/H2O over 5 min)=0.95 min.

1. customFirst, N-benzyl-pyrrolidine-3-methanol was prepared
2. additionThis solution was added to a 0° C.
3. additionAfter addition
4. temperaturethe mixture was refluxed for 1 hr
5. temperaturecooled with an ice bath
6. customTo quench
7. customthe reaction, sodium sulfate decahydrate
8. additionwas added
9. filtrationAfter filtration
10. customthe filtrate was collected
11. concentrationconcentrated to dryness