2-Methoxyethylamine → HCID 178495985、化合物

関与物質

反応条件

反応手順

4-Amino-N-hydroxy-1,2,5-oxadiazole-3-carboximidoyl chloride (200.0 g, 1.23 mol) was mixed with ethyl acetate (1.2 L). At 0-5° C. 2-methoxyethylamine [Aldrich, product #143693] (119.0 mL, 1.35 mol) was added in one portion while stirring. The reaction temperature rose to 41° C. The reaction was cooled to 0-5° C. Triethylamine (258 mL, 1.84 mol) was added. After stirring 5 min, LCMS indicated reaction completion. The reaction solution was washed with water (500 mL) and brine (500 mL), dried over sodium sulfate, and concentrated to give the desired product (294 g, 119%) as a crude dark oil. LCMS for C6H12N5O3 (M+H)+: m/z=202.3. 1H NMR (400 MHz, DMSO-d6): δ 10.65 (s, 1 H), 6.27 (s, 2 H), 6.10 (t, J=6.5 Hz, 1 H), 3.50 (m, 2 H), 3.35 (d, J=5.8 Hz, 2 H), 3.08 (s, 3 H).

情報源と証拠