Thieno[2,3-d]pyrimidinyl hydroxamic acid derivatives and uses thereof
A pyrimidine hydroxamic acid, 3-d technology, applied in the field of antitumor drugs, can solve problems such as single effect, achieve good therapeutic effect, novel structure, and increase the effect of cytotoxic T cell infiltration
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[0048] The compound of the present invention can be prepared by conventional chemical synthesis methods, specifically, the following process flow is used for synthesis:
[0049]
[0050] Reagents and conditions: (a) NCCH 2 CO 2 Et, S 8 ,Et 3 N, EtOH, reflux, 12h; (b) DBU, THF, reflux, 24h; (c) CH 3 OH, NaOH, 30min; (d) DCC / HOBt, DCM, 24h; (e) ethyl chloroformate, N-methylmorpholine, 1,4-dioxane, 15min, then NH 2 OH, CH 3 OH, 20min; (f) compound 2a-e, HCl-1,4-dioxane, 25°C, 48h.
Embodiment 1
[0052] Example 1 N-(2-aminophenyl)-4-(2,6-dimethyl-4-(7-methyl-4-oxo-3,4,5,6,7,8-hexa Preparation of hydropyridin[4',3':4,5]thiophene[2,3-d]pyrimidin-2-yl)phenoxy)butyramide (8b)
[0053]
[0054] Reaction a: Preparation of ethyl 2-amino-6-methyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate (2a)
[0055] Mix N-methylpiperidone (4.90 g, 50 mmol), ethyl cyanoacetate (5.66 g, 100.0 mmol), triethylamine (10 mL) and sublimed sulfur (1.60 g, 50.0 mmol) in 100 mL of absolute ethanol The reaction was refluxed for 12 hours, the reaction solution was concentrated, the residue was extracted with water and ethyl acetate, the organic layer was separated and concentrated, and 2a was recrystallized with 100ml of ethanol, the yield was 79%, light yellow powder. 1 H NMR (400MHz, DMSO-d 6 )δ7.23(s,2H,NH 2 ), 4.15 (q, J=7.2Hz, 2H, OCH 2 CH 3 ),3.22(t,J=2.0Hz,2H,N-CH 2 -Thiophene), 2.66 (t, J=5.2Hz, 2H, N-CH 2 -CH 2 ),2.53(t,J=6.0Hz,2H,N-CH 2 -CH 2 ),2.29(s,3H,N-CH 3 ), 1.2...
Embodiment 2
[0064] Example 2 N-(2-aminophenyl)-2-(2,6-dimethyl-4-(7-methyl-4-oxo-3,4,5,6,7,8-hexa Preparation of hydropyridin[4',3':4,5]thiophene[2,3-d]pyrimidin-2-yl)phenoxy)acetamide (8a)
[0065]
[0066] Referring to the preparation method of Example 1, the raw material 4-bromobutyrate methyl ester in reaction b was changed to 4-bromoacetate methyl ester to obtain compound 8a.
[0067] Pale yellow solid, yield 35%. mp:243.7-245.8℃. 1 H NMR (400MHz, DMSO-d 6 )δ12.39(brs,1H,Pyrimidine-H),9.80(s,1H,CONH),8.15(s,1H,Ar-H),8.02(d,J=7.6Hz,1H,Ar-H), 7.92(s, 2H, Ar-H), 7.72(d, J=7.6Hz, 1H, Ar-H), 7.57(t, J=7.6Hz, 1H, Ar-H), 7.19(d, J=7.8 Hz,1H,Ar-H),6.98(t,J=7.6Hz,1H,Ar-H),6.80(d,J=8.0Hz,1H,Ar-H),6.61(t,J=7.6Hz, 1H,Ar-H),4.95(s,4H,O-CH 2 ,NH 2 ),3.56(s,2H,N-CH 2 -Thiophene), 2.97(t, J=5.6Hz, 2H, N-CH 2 -CH 2 ), 2.67(t, J=5.6Hz, 2H, N-CH 2 -CH 2 ),2.38(s,3H,N-CH 3 ),2.35(s,6H,2Ar-CH 3 ). 13 C NMR (100MHz, DMSO-d 6 )δ165.61,164.26,160.45,158.33,153.33,143.66,137.97,135.27,131....
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