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. temperatureand then cooled 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