反应 #1152228
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07345067B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of (2-fluoro-4-nitro-phenoxy)-acetic acid ethyl ester (17.0 g, 55.92 mmol) in EtOH (330 ml) and aqueous 1M HCl (55.92 ml, 55.92 mmol) was hydrogenated in the presence of 10% Pd/C (1.7 g) for 2 days. After removal of the catalyst the reaction was evaporated and treated with water/Et2O (3×), the aqueous phase was treated with NaHCO3 and extracted with Et2O (3×). The organic phases were washed with aqueous 10% NaCl, dried (Na2SO4) and evaporated to give 5.39 g (45%) of (4-amino-2-fluoro-phenoxy)-acetic acid ethyl ester as a brown crystallin residue, MS: 213 (M+). After removal of the catalyst the reaction was evaporated treated with water/Et2O (3×) the aqueous phase was treated with NaHCO3 extracted with Et2O (3×) The organic phases were washed with aqueous 10% NaCl dried (Na2SO4) evaporated
来源 ID: ord-8ae497ecb8e8456a9da5e19ce448c878