反应 #3713747
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05484946
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of ethyl 3-aminobutyrate hydrochloride (4.5 g, 26.8 mmol) in 27 mL of 1N NaOH was extracted 2X with EtOAc. The organic fraction was dried (Na2SO4) and concentrated under reduced pressure. Recrystallization of the residue 3X from EtOAc afforded 1.93 g (51%) of product as a single chiral diastereomer as determined by NMR spectroscopy (m.p. 125°-125° C.). 1H-NMR (300 MHz, CDCl3 ) δ1.00 (d, J=7 Hz, 3H), 1.27 (t, J=7 Hz, 3H, 2.23-2.45 (m, 2H), 3.13 (m, 1H), 4.13 (q, J=7 Hz, 2H), 4.85 (s, 1H), 7.17-7.33 (m, 3H), 7.41 (d, J=8 Hz, 2H). Anal. calc'd. for C14H21NO5 : C, 59.35; H, 7.47; N, 4.94. The organic fraction was dried (Na2SO4) concentrated under reduced pressure Recrystallization of the residue 3X from EtOAc
来源 ID: ord-9cb18b6c9a944c9cb78ff3d0585264e0