Synthetic Route of 383-62-0,Some common heterocyclic compound, 383-62-0, name is Ethyl 2-chloro-2,2-difluoroacetate, molecular formula is C4H5ClF2O2, 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.
Step 3 – Synthesis of l-(3-(difluoromethoxy)-lH-pyrazol-l-yl)ethanone [0228] To a 250 mL round-bottom flask was added l-(3-hydroxy-lH-pyrazol-l- yl)ethanone (5.0 g, 39.65 mmol, 1.00 equiv), N,N-dimethylformamide (50.0 mL), potassium carbonate (11.0 g, 79.02 mmol, 2.00 equiv) and ethyl 2-chloro-2,2-difluoroacetate (7.5 g, 47.31 mmol, 1.20 equiv). The resulting solution was stirred for 12 h at 60 C, then diluted with water. The resulting mixture was extracted with ethyl ether (3x) and the combined organic layers washed with water, dried over anhydrous sodium sulfate and concentrated under vacuum. The crude product was applied onto a silica gel column eluting with ethyl ether/hexanes (0: 100 to 1 : 1) to afford the title compound as colorless oil. 1H-NMR (400 MHz, CDC13): delta 8.15 (d, 1H), 7.02 (t, 1H), 6.14 (d, 1H), 2.62 (s, 3H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2-chloro-2,2-difluoroacetate, its application will become more common.
Reference:
Patent; MERCK SHARP & DOHME CORP.; LYCERA CORPORATION; AICHER, Thomas D.; VAN HUIS, Chad A.; MACLEAN, John K.; ANDRESEN, Brian M.; BARR, Kenneth J.; BIENSTOCK, Corey E.; ANTHONY, Neville J.; DANIELS, Matthew; LIU, Yuan; WHITE, Catherine M.; LAPOINTE, Blair T.; SCIAMMETTA, Nunzio; SIMOV, Vladimir; TROTTER, Wesley, B.; LIU, Kun; WO2015/95788; (2015); A1;,
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