2-Fluoro-5-nitrobenzonitrile → 5-Amino-2-fluorobenzonitrile

To a solution of 2-fluoro-5-nitrobenzonitrile (2.0 g, 12 mmol) in ethyl acetate(50 mL) was added stannous chloride (27.0 g, 120 mmol). The reaction mixture was stirred at reflux 1.5 h, then cooled to room temperature. Partitioned between ethyl acetate (150 mL) and saturated sodium bicarbonate(150 mL). Organic phase was separated and washed with water (5×75 mL), brine (75 mL); dried over sodium sulfate (anhy.); filtered and concentrated to give 2-fluoro-5-aminobenzonitrile (1.4 g) as pure compound.

1. temperatureat reflux 1.5 h
2. customPartitioned between ethyl acetate (150 mL) and saturated sodium bicarbonate(150 mL)
3. customOrganic phase was separated
4. washwashed with water (5×75 mL), brine (75 mL)
5. dry with materialdried over sodium sulfate (anhy.)
6. filtrationfiltered
7. concentrationconcentrated

ORDレコード

ord-8478ae9ce00f4aafb8ce937a724cad71

出典データセット

uspto-grants-2000_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06020357