C4-modified oleanolic acid derivatives for inhibition of IL-17 and other uses
A chemical compound, atomic technology, applied in biology and medicine, which can solve the problems of patients who cannot relieve symptoms, significant side effects, and life-threatening problems
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example 1
[1033] Example 1: Synthesis and Characterization
[1034] Process 1
[1035]
[1036] Reagents and conditions: a) NH 2 OH·HCl, NaOAc, CH 2 Cl 2 , MeOH, 60°C; b) AcOH, Ac 2 O; PhI(OAc) 2 , Pd(OAc) 2 , ClCH 2 CH 2 Cl, 60-80°C, 43% from 1; c) K 2 CO 3 , MeOH, room temperature; d) sodium bisulfite, EtOH aqueous solution, 80 ° C, 73% from 3; e) Jones reagent, acetone, 0 ° C; 80-120 ° C, vacuum, 81%; f) HCO 2 Et, NaOMe, MeOH, THF, 0°C-room temperature; NH 2 OH·HCl, aqueous EtOH, 55°C, 44%; g) NaOMe, MeOH, THF, 55°C, 51%; h) DBDMH, DMF, 0°C; Py, 55°C, 80%.
[1037] Process 2
[1038]
[1039] Reagents and conditions: a) HCO 2 Et, NaOMe, MeOH, 0°C; NH 2 OH·HCl, EtOH aqueous solution, 55°C, 57%; b) Jones reagent, acetone, 0°C-room temperature, 88%; c) TMSCHN 2 、Et 2 O, toluene, MeOH, 0°C, 84%; d) NaOMe, MeOH, 55°C, quantitative yield; e) DBDMH, DMF, 0°C; Py, 55°C, 77%.
[1040] Process 3
[1041]
[1042] Reagents and conditions: a) i) Jones reagent, acetone,...
example 2
[1335] Example 2: Bioactive Methods and Materials
[1336] A. Analysis of Nitric Oxide Production and Cell Viability
[1337] RAW 264.7 mouse macrophages were seeded in triplicate at a density of 30,000 cells per well in 96-well culture dishes in RPMI 1640+0.5% FBS and incubated at 37°C and 5% CO 2 Grow in a moist atmosphere. The next day, cells were pretreated with DMSO (vehicle) or test compounds (concentration range 0.4-200 nM or 2-1000 nM) for 2 hours, followed by recombinant mouse IFNγ (R&D Systems) for 24 hours . The nitric oxide concentration in the medium was determined using the Griess reagent system (Promega). Cell viability was determined using WST-1 reagent (Roche). Values of test compound samples were normalized to values of DMSO / IFNγ-treated samples. IC was determined based on inhibition of IFNγ-induced nitric oxide production normalized to cell viability 50 value.
[1338] B. AREc32 luciferase reporter assay
[1339] The AREc32 luciferase reporter as...
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