Lithium Hydroxide → 2-Methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid

To a solution of 1.48 g (6.52 mmol) 2-Methyl-N-(2,2,2-trifluoro-ethyl)-malonamic acid ethyl ester in 40 ml of tetrahydrofurane, 20 ml of water and 1.09 g (26 mmol) of lithium hydroxide were added and the mixture was stirred overnight at room temperature. After concentration in vacuo water (50 ml) was added and the mixture was extracted with dichloromethane (three times 30 ml). The aqueous phase was acidified with 8 N hydrochloric acid and extracted with dichloromethane (four times 30 ml). The combined organic layers from the second extraction were dried (MgSO4) and evaporated in vacuo to give 1.09 g (84%) of the title compound as a white solid.

1. concentrationAfter concentration in vacuo water (50 ml)
2. additionwas added
3. extractionthe mixture was extracted with dichloromethane (three times 30 ml)
4. extractionextracted with dichloromethane (four times 30 ml)
5. extractionThe combined organic layers from the second extraction
6. dry with materialwere dried (MgSO4)
7. customevaporated in vacuo

ORD record

ord-1f054652294840449f82e344472d5240

Source dataset

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07160875B2