In
a 2 L three-necked flask, add 36.4 g (0.1 mol) of solid material SM1,
dissolve with 360ml butanone, then add 19.9 g Intermediate C (0.105
mol), 8.3g HOPO (0.075 mol) and stir for 10min, then add 38.7 g DIPEA
(0.3 mol), stirred for 10min, then added 26.6 g EDCI (0.15 mol), reacted
at 20-25
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°C for 16-18 h, the raw material point basically
disappeared in TLC, and phosphoric acid aqueous solution (85%, 0.15 mol,
47.5 g was added to the reaction solution) ) and 360 ml of saturated
sodium chloride solution, stirred for 30 min, left to stand for
stratification, let go of the lower water layer, add 360 ml of sodium
chloride solution and 360 ml of isopropyl acetate solution to the
organic layer, extract and separate liquids, and concentrate the organic
layer to obtain 45.6 g of crude product, the yield is 91.3%.
In the
there-necked flask of 2 L, add crude product (50 g, 0.1 mol), 500 ml
isopropyl acetate, be heated to 65-70°C after solids are all dissolved,
under this temperature condition, add the n-heptane of 750 ml , heat
preservation and stirring 6-7 h, separate out a large amount of solid,
be cooled to room temperature, filter, filter cake is washed with the
organic solvent F of 300 ml (wherein, organic solvent F is that
isopropyl acetate and n-heptane are mixed by volume ratio of 1:1 mixed
solution), and dried to obtain 46.2 g of pure product with a yield of
92.3%.
