Novel HCV virus NS3/4A inhibitor synthesizing intermediate and synthesis method
A synthetic method and inhibitor technology, applied in the direction of organic chemistry, can solve the problems of low product yield and high raw material cost, and achieve the effect of high synthetic yield, low raw material cost and reduced raw material input
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Embodiment 1
[0048]
Embodiment 2
[0051]
[0052] Add CCl to the 5L reaction flask 4 1.5L, add compound IV 120g, add 2g AIBN, add NBS1.1eq in batches, under the protection of nitrogen, heat up to 85°C and reflux reaction overnight. TLC detects that the reaction of raw materials is complete. The reaction solution was cooled to room temperature, poured into an aqueous solution of sodium thiosulfate, separated the organic phase, extracted the aqueous phase with MTBE, washed the organic phase three times with aqueous sodium thiosulfate, washed twice with saturated aqueous sodium chloride, and anhydrous Dry over sodium sulfate and concentrate. The residue was separated and purified by column chromatography, eluent PE (petroleum ether): EA (ethyl acetate) = 40:1-20:1 to obtain the crude product, and then the crude product was distilled under reduced pressure, 2 Torr, external temperature 168°C, internal temperature 120°C. 110 g of compound III was obtained as a colorless liquid.
Embodiment 3
[0054]
[0055] The compound III obtained in Example 2 was added to the freshly prepared 10M ammonia methanol solution, and stirred overnight. When no white solid is precipitated, filter and drain to obtain 60 g of off-white product. 1 H NMR (400MHz, DMSO) δ8.85(s, 1H), 7.84(d, J=7.8Hz, 1H), 7.73(d, J=7.4Hz, 1H), 7.49(t, J=7.6Hz, 1H ),4.34(s,2H).
[0056] NMR identification of this type of white product was confirmed as compound Ⅱ.
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