Treatment agent for inflammatory bowel disease
A technology for inflammatory bowel disease and treatment agent, which can be used in anti-inflammatory agents, allergic diseases, non-central analgesics, etc., and can solve problems such as unknown antecedent drugs.
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Embodiment 1
[0213] Example 1: Formulation example of tablet
[0214]
[0215] The active ingredient is pulverized to a particle size of 70 μm or less, starch, lactose and carboxymethylcellulose calcium are added thereto, and thoroughly mixed. Add 10% starch slurry into the above mixed powder and stir and mix to prepare granules. After drying, adjust the particle size to about 1000 μm, mix talc powder and magnesium stearate therein, and press into tablets.
preparation example 1
[0217] 3-(4-fluorophenyl)-5-(phenylacetylamino)-4-(4-pyrimidinyl)isoxazole
[0218] a: Synthesis of dimethyl-[(E)-2-(4-pyrimidinyl)vinyl]amine
[0219] A mixture of 10 g of 4-methylpyrimidine and 38 g of N,N-dimethylformamide dimethyl acetal (DMFDMA) and 46.6 g of DMF was stirred at 140° C. for 24 hours in a sealed tube. After cooling the reaction solution, the solvent was distilled off under reduced pressure to obtain 15.08 g of the title compound as brown crystals (95% yield).
[0220] 1 H-NMR (CDCl 3 )δ: 8.73 (bs, 1H), 8.22 (d, J=5.5Hz, 1H), 7.77 (d, J=12.9Hz, 1H), 6.72 (dd, J=5.5Hz, 12.9Hz, 1H), 5.00 (d, J=12.9Hz, 1H), 2.96(s, 6H)
[0221] b: Synthesis of 4-pyrimidinylacetonitrile
[0222] 9.48 g of hydroxylamine-O-sulfonic acids were added to 70 mL of aqueous solutions of 5 g of dimethyl-[(E)-2-(4-pyrimidinyl)vinyl]amine, and it stirred at 50 degreeC for 30 minutes. Under ice-cooling, saturated aqueous sodium bicarbonate solution was added to make the reaction s...
preparation example 2
[0233] 5-[(2-Chlorophenyl)acetylamino]-3-(4-fluorophenyl)-4-(4-pyrimidinyl)isoxazole (Compound number: B-1)
[0234] Using 2-chlorophenylacetyl chloride instead of phenylacetyl chloride, the title compound was synthesized in the same manner as in Preparation 1-d.
[0235] 1 H-NMR (CDCl 3 )δ: 11.45(bs, 1H), 8.54(s, 1H), 8.38(d, J=5.7Hz, 1H), 7.55~7.38(m, 6H), 7.20(t, J=8.7Hz, 2H), 6.75(dd, J=1.3Hz, 5.7Hz, 1H), 4.06(s, 2H)
[0236] Mass spectrum, m / e: 408 (M + ), 240 (base peak)
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