Benzene, 2-fluoro-4-methyl-1-nitro- → 3-(5-Methyl-2-nitro-phenylamino)-hexanoic acid ethyl ester

To a solution of 3-Fluoro-4-nitrotoluene (1.0 g, 6.5 mmol) in DMF (5 mL) were: 3-Amino-hexanoic acid ethyl ester hydrochloride (1.3 g, 6.7 mmol) and DIPEA (2.2 mL, 12.9 mmol). The reaction mixture was stirred at room temperature for 48 h. The reaction mixture was then diluted with ethyl acetate and washed with water (×4). The organic phase was then dried over Na2SO4 and concentrated. The resulting residue was purified by Combiflash using hexane and ethyl acetate (10% gradient) as an eluent to afford 1.4 g of the desired product as orange oil.

1. washwashed with water (×4)
2. dry with materialThe organic phase was then dried over Na2SO4
3. concentrationconcentrated
4. customThe resulting residue was purified by Combiflash

ORD-Eintrag

ord-836a387586724ecdb604e6f9f56de0bf

Quelldatensatz

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09150556B2