Dimethylformamide → HCID 23121940, 화합물

To 1,1-dimethylethyl N-(2-oxoethyl)carbamate (2.0 g, 13 mmol) were added N,N-dimethylformamide (50 mL), tetrahydrofuran (50 mL), 1,2,3,6-tetrahydropyridine (1.2 mL, 13 mmol) and sodium triacetoxyborohydride (5.3 g, 25 mmol), and the mixture was stirred at room temperature for 14 hours. To the reaction solution was added ethyl acetate, and the resulting mixture was washed with a 0.5 M aqueous sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate to ethyl acetate:methanol=8:2) and further purified with amino silica gel column chromatography (hexane:ethyl acetate=9:1 to ethyl acetate) to obtain the title compound (1.2 g, yield 41%).

1. washthe resulting mixture was washed with a 0.5 M aqueous sodium hydrogen carbonate solution
2. dry with materialdried over anhydrous magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified with silica gel column chromatography (ethyl acetate to ethyl acetate:methanol=8:2)
5. customfurther purified with amino silica gel column chromatography (hexane:ethyl acetate=9:1 to ethyl acetate)

ORD 기록

ord-b6a55f42ad5f4a0094f6f6359df36e95

출처 데이터셋

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07795267B2