Water → HCID 86609568, compound

8-Aminocaprylic acid (970.3 mg, 6.1 mmol) was dissolved in tert-butylalcohol (14.7 ml), 5N NaOH (1.44 ml, 6.1 mmol) was added thereto, and the mixture was stirred at room temperature for 10 minutes. Di-tert-butyl-dicarbonate (1.46 g, 6.7 mmol) dissolved in tert-butylalcohol (10 ml) was added thereto and stirred at room temperature for 24 hours. Then, water (10 ml) was added thereto and the mixture was concentrated under a reduced pressure, cooled to 0° C., and then, 2N H2SO4 was added thereto dropwise until pH of the mixture became 2. The resultant was extracted with ethyl acetate, the extract was washed with H2O, dried over MgSO4 and concentrated. The concentrate was purified using column chromatography (ethyl acetate:toluene:acetic acid=20:10:0.3) to obtain the title compound (1.78 g) as a white solid.

1. additionwas added
2. stirringstirred at room temperature for 24 hours
3. concentrationthe mixture was concentrated under a reduced pressure
4. temperaturecooled to 0° C.
5. addition2N H2SO4 was added
6. extractionThe resultant was extracted with ethyl acetate
7. washthe extract was washed with H2O
8. dry with materialdried over MgSO4
9. concentrationconcentrated
10. customThe concentrate was purified

ORD record

ord-8c1c913d638b4e39aafdeeb67e893d95

Source dataset

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07589072B2