Benzomorpholone derivatives and their preparation and use
A technology of benzomorpholone and derivatives, which is applied in the field of benzomorpholone derivatives and their preparation, and can solve problems such as no drugs on the market and single structure type of small molecule inhibitors
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Embodiment 1
[0088] Example 1 Preparation of N-(2-methyl-2H-1,4-benzomorpholine-3(4H)-one-7-yl)benzenesulfonamide (compound 1)
[0089]
[0090] (1) Synthesis of 2-methyl-7-nitro-2-hydrogen-1,4-benzomorpholin-3(4-hydrogen)-one:
[0091]
[0092] Add 125 mM potassium carbonate to 100 mL of dried DMF (N,N-dimethylformamide), add 50 mM 2-amino-5-nitrophenol to it and stir at room temperature for 1 h until it is completely dissolved. Under the condition of ice bath, a DMF solution of 50 mM ethyl 2-bromopropionate was slowly added dropwise. Half an hour later, the reaction solution was slowly raised to room temperature, and reacted at 90°C for 12h. After the reaction solution is cooled, part of the solvent is evaporated under reduced pressure. Slowly add 300-500mL of ice water under stirring conditions, and solids precipitate out. Stir under ice bath conditions for half an hour, filter, and vacuum-dry the filter cake to obtain a relatively pure intermediate product, which is brown. Powd...
Embodiment 2
[0102] Example 2 Preparation of 4-methyl-N-(2-methyl-2H-1,4-benzomorpholine-3(4H)-one-7-yl)benzenesulfonamide (compound 2)
[0103]
[0104] Using p-toluenesulfonyl chloride as raw material, it was prepared according to the preparation method of Example 1.
[0105] 1 HNMR (400MHz, DMSO-d6) δ10.55(s, 1H), 10.06(s, 1H), 7.60(d, J=8.2Hz, 2H), 7.35(d, J=8.1Hz, 2H), 6.75- 6.66(m,2H),6.65(s,1H),4.59(q,J=6.7Hz,1H),2.34(s,3H),1.36(d,J=6.8Hz,3H); 13 C NMR (101MHz, DMSO-d6) δ166.36(s), 143.16(s), 142.95(s), 136.47(s), 132.82(s), 129.63(s), 126.67(s), 124.19(s) , 115.74(s), 114.66(s), 109.06(s), 72.62(s), 20.92(s), 15.95(s). ESI-MS:m / z:355.1[M+Na] + .
Embodiment 3
[0106] Example 3 Preparation of 4-chloro-N-(2-methyl-2H-1,4-benzomorpholin-3(4H)-one-7-yl)benzenesulfonamide (compound 3)
[0107]
[0108] Using p-chlorobenzenesulfonyl chloride as a raw material, it was prepared according to the preparation method of Example 1.
[0109] 1 HNMR(400MHz,DMSO-d6)δ10.52(s,1H),10.44(s,1H),7.99(d,J=7.4Hz,1H),7.63(d,2H),7.51(t,J=6.2 Hz,1H),6.69(d,J=11.2Hz,3H),4.62-4.54(m,1H),1.34(d,J=6.7Hz,3H); 13 C NMR (101MHz, DMSO-d6) δ166.31(s), 143.00(s), 134.64(s), 131.94(s), 131.55(s), 115.77(s), 108.40(s), 72.62(s) ,15.95(s). ESI-MS:m / z:375.5[M+Na] + .
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