Aluminium lithium hydride → HCID 50988607, compound

Temperature

-10 °C

To a solution of 4-(2,2,2-trifluoroethyl)pyrrolidin-2-one a1-10 (4.0 g, 23.9 mmol, 1 eq) in freshly distilled THF, LiAlH4 (2.27 g, 60 mmol, 2.5 eq) is added carefully at 0° C. After completion of the addition, the mixture is heated at reflux for 1.5 h in a flask equipped with a condenser cooled at −10° C. The reaction mixture is then carefully quenched with water at 0° C. and filtered on a pad of celite/MgSO4. The filtrate is concentrated under reduced pressure at room temperature to afford 2.82 g of 3-(2,2,2-trifluoroethyl)pyrrolidine a1-11.

1. additionAfter completion of the addition
2. temperaturethe mixture is heated
3. temperatureat reflux for 1.5 h in a flask
4. customequipped with a condenser
5. customThe reaction mixture is then carefully quenched with water at 0° C.
6. filtrationfiltered on a pad of celite/MgSO4
7. concentrationThe filtrate is concentrated under reduced pressure at room temperature

ORD record

ord-762834037d36452896066e406a33e206

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09067930B2