Sodium hydride → HCID 66717596, 화합물

A solution of 3-amino-4-fluorophenol (4.1 g) in N,N-dimethylformamide (15 mL) was added dropwise to a stirred suspension of sodium hydride (60% in oil, 1.3 g) in N,N-dimethylformamide (35 mL) at 0° C. The mixture was stirred a room temperature for 30 minutes, cooled 0° C. and then (R)-2-chloropropionic acid methyl ester (4.0 g) was added in one portion. The resulting mixture was stirred at room temperature overnight and then treated with saturated aqueous ammonium chloride solution. The mixture was extracted with ethyl acetate and the combined extracts, washed with saturated aqueous sodium chloride solution and then dried over magnesium sulfate. The solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel, eluting with a mixture of dichloromethane and ethyl acetate (1:0 to 3:2 by volume) to give the mixture of title compounds as golden oil, 2.5 g.

1. temperaturecooled 0° C.
2. stirringThe resulting mixture was stirred at room temperature overnight
3. extractionThe mixture was extracted with ethyl acetate
4. washthe combined extracts, washed with saturated aqueous sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. customThe solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel
7. washeluting with a mixture of dichloromethane and ethyl acetate (1:0 to 3:2 by volume)
8. customto give
9. additionthe mixture of title compounds as golden oil, 2.5 g

ORD 기록

ord-73de70f69d1346b78617fb468d731c1e

출처 데이터셋

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07858640B2