Compounds capable of inhibiting ErbB/HDAC and preparation method thereof, and pharmaceutical composition comprising compounds and application thereof
A technology of compounds and solvates, applied in the field of medicine, can solve the problems of increased acetylation level and degradation of HSP90
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Embodiment 1
[0070] Example 1: (Compound 1) Preparation
[0071] Step 1a, preparation of 6-iodoquinazolin-4-one (102)
[0072] Formamide (13.7 g, 304 mmol) and 2-amino-5-iodobenzoic acid (compound 101, 20 g, 76.0 mmol) were reacted at 190° C. for 4 hours. After the reaction, 100 mL of methanol was added, the reaction solution was filtered, the filter cake was rinsed with methanol, and compound 102 was obtained after drying. Yield 80.6%.
[0073] The confirmed data of the compound structure are:
[0074] 1 H NMR (400MHz, DMSO) δ12.42(s, 1H), 8.42–8.34(m, 1H), 8.14(d, J=1.4Hz, 1H), 8.12–8.05(m, 1H), 7.46(t, J=6.8Hz,1H).
[0075] Step 1b, preparation of 4-chloro-6-iodoquinazoline (103)
[0076] Compound 102 (14.4 g) was dissolved in thionyl chloride (50 ml), 1 mL of catalytic amount of anhydrous DMF was added, and the reaction was refluxed for 4 hours. After the reaction, excess thionyl chloride was distilled off under reduced pressure to obtain compound 103. Yield 92.4%.
[0077] ...
Embodiment 2
[0105] Example 2: (Compound 2) Preparation
[0106] Compound 2 was prepared according to the steps of Example 1, except that:
[0107] 1. Preparation of 7-azidoheptanoic acid (108b)
[0108] 107a in step 1f in Example 1 was replaced with 7-bromoheptanoic acid (107b) for reaction. Yield 81.5%.
[0109] The confirmed data of the compound structure are:
[0110] 1 H NMR (400MHz, CDCl 3 )δ11.36(s,1H),3.27(t,J=6.9Hz,2H),2.36(t,J=7.4Hz,2H),1.70–1.56(m,4H),1.45–1.34(m,4H ).
[0111] 2. Preparation of 7-azido-N-((tetrahydropyran-2-substituted) oxy)heptanamide (109b)
[0112] 108a in step 1g in Example 1 was replaced by 108b for reaction. Yield 89.8%.
[0113] The confirmed data of the compound structure are:
[0114] 1 H NMR (400MHz, CDCl 3 )δ8.76(s,1H),4.89(s,1H),3.95(d,J=9.4Hz,1H),3.63(m,1H),3.26(t,J=6.9Hz,3H),2.19– 1.76(m,4H),1.73–1.48(m,8H),1.45–1.29(m,4H).
[0115] 3. Preparation of 7-(4-(4-((3-chloro-4-fluorophenylamino)quinazoline-6-substituted)-1 hydrogen-1,2,3...
Embodiment 3
[0123] Example 3: (Compound 3) Preparation
[0124] Compound 3 was prepared according to the steps of Example 1, except that:
[0125] 1. Preparation of N-(3-chloro-2-fluorophenyl)-6-iodoquinazolin-4-amine (104b)
[0126] The 3-chloro-4-fluoroaniline in step 1c in Example 1 was replaced with 3-chloro-2-fluoroaniline for the reaction. Yield 95.1%.
[0127] The confirmed data of the compound structure are:
[0128] 1 H NMR (400MHz,DMSO)δ12.26(s,1H),9.48–9.34(m,1H),8.97(d,J=2.8Hz,1H),8.41(dd,J=8.8,1.3Hz,1H) ,7.87–7.77(m,1H),7.66(t,J=7.4Hz,1H),7.58–7.50(m,1H),7.37(t,J=8.1Hz,1H).
[0129] 2. Preparation of N-(3-chloro-2-fluorophenyl)-6-ethynylquinazolin-4-amine (106b)
[0130] The reaction was carried out by replacing 104a in step 1d / e of Example 1 with 104b. Yield 69.3%.
[0131] The confirmed data of the compound structure are:
[0132] 1 H NMR(400MHz,DMSO)δ10.13(s,1H),8.69(s,1H),8.55(s,1H),7.90(d,J=8.5Hz,1H),7.79(d,J=8.6Hz ,1H),7.52(t,J=7.4Hz,2H),7.29(t,J=8.0Hz,1H),...
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