Some common heterocyclic compound, 96-30-0, name is 2-Chloro-N-methylacetamide, molecular formula is C3H6ClNO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of 2-Chloro-N-methylacetamide
To a solution of bumetanide 32-1 (2.5 g, 6.86 mmol) in N,N-Dimethylformamide (25 mL) were added tri ethyl amine (1.4 mL, 10.2 mmol), Nal (1 .13 g, 7.5 mmol) and 2-Chloro-N-methyl-acetamide 32-2 (0.88 g, 8.23 mmol) at 0-5 C. The reaction mixture was allowed to stir at 50 C for lOh. The reaction mass was diluted with ethyl acetate (300 mL) and washed with water (2 X 100 mL), dried over sodium sulfate and concentrated under reduced pressure. The crude product obtained upon evaporation of volatiles was purified by silica gel (230-400 mesh) column chromatography to give product Compound 25 as an off white solid 1.8 g (60%). 1H NMR (400 MHz, DMSO-de) d 8.09 (q, 1H), 7.74 (d, J = 2 Hz, 1H), 7.47-7.35 (m, (0926) 3H), 7.27 (t, j = 8 Hz, 2H), 7.02 (t, J = 8 Hz, i l l), 6.85 (d, J = 8 Hz, 2H), 5.18 (t, 1H), 4.73 (s, 21 1 > 3.12-3.01 (m, 2H), 2.64 (d, 31 1). 1.37 (quintet, 2H), 1.11 (sextet, 2H), 0.77 (t, 3H); MS m/z [M+H]+ 436.7.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 96-30-0, its application will become more common.
Reference:
Patent; GRAYBUG VISION, INC.; YANG, Ming; BAUMAN, John, G.; ZHANG, Jinzhong; HOANG, Nu; CLELAND, Jeffrey, L.; (355 pag.)WO2019/210215; (2019); A1;,
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