Lithium hydroxide, monohydrate → HCID 69040656, compound

A solution of 75 mg (0.2 mmol) of (2S)-2-fluoro-2-methyl-N-((S)-5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamic acid ethyl ester in 1 ml of tetrahydrofurane was treated for 2 h at room temperature with a solution of 8 mg (0.2 mmol) of lithium hydroxide monohydrate in 0.5 ml of water. For the working-up, the tetrahydrofurane was evaporated under reduced pressure and the remaining aqueous layer was extracted twice with 10 ml of diethylether. The combined organic layers were washed with 5 ml of water and, thereafter, the combined aqueous layers were acidified with 0.025 ml of hydrochloric acid (25%). Thereupon, the aqueous layer was extracted three times with 15 ml of ethyl acetate. The organic layers were washed with 15 ml of a saturated solution of sodium chloride, then combined, dried over sodium sulphate, and evaporated under reduced pressure. There were obtained 69 mg (99% of theory) of the title compound as a white foam;

1. customthe tetrahydrofurane was evaporated under reduced pressure
2. extractionthe remaining aqueous layer was extracted twice with 10 ml of diethylether
3. washThe combined organic layers were washed with 5 ml of water
4. extractionThereupon, the aqueous layer was extracted three times with 15 ml of ethyl acetate
5. washThe organic layers were washed with 15 ml of a saturated solution of sodium chloride
6. dry with materialdried over sodium sulphate
7. customevaporated under reduced pressure

ORD record

ord-e4b2377746c94245b78f743e4f36c2fa

Source dataset

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07160875B2