5-substituted methylene imidazolidine-2, 4-diketone derivative as well as pharmaceutical composition and application thereof
A technology of imidazolidine and benzylidene, which is applied in the field of organic chemical drug synthesis, and can solve unseen problems
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Embodiment 1
[0107] Preparation of 5-Hydroxybenzylmethyleneimidazolidine-2,4-dione (Ⅱ)
[0108]
[0109] Add 6.11 g (50 mmol) of hydroxybenzaldehyde and 5.5 g (55 mmol) of imidazolidine-2,4-dione into a 250 mL round bottom flask, add 10 mL of piperidine, install a reflux condenser and a drying tube above the flask, Place the flask in an oil bath to make the reaction solution level with the oil bath surface, heat to 130°C and keep for 30 minutes; generate a large number of bubbles and slightly boil; add 200 mL of distilled water at 60°C after cooling, stir with a glass rod until the solid dissolves, and obtain a red color solution and yellow flocculent insoluble matter, filtered to remove the insoluble matter, after the filtrate was cooled to room temperature, the filtrate was transferred to a beaker, and 20 mL of 10 N HCl solution was added dropwise while stirring; after standing at room temperature for 12 h, the The yellow precipitate was obtained by suction filtration through a Schnei...
Embodiment 2
[0114]
[0115] p-Chlorobenzyl chloride and 5-(4-p-hydroxybenzylidene) imidazolidine-2,4-dione reaction steps: Mixed 5-[4-p-hydroxybenzylidene] imidazolidine-2,4- Diketone (4.08g, 20mmol), p-chlorobenzyl chloride (3.24g, 20mmol), K 2 CO 3 (2.76g, 20mmol) and acetone (120mL) were refluxed for 24 h, TLC detected that the reaction of the raw materials was complete, and the reaction was stopped; after cooling, the inorganic salt was removed by filtration; I-1: white solid (0.46g, 14.00 %), m.p.255~258℃; I-2: light yellow solid (0.62 g, 27.15%), m.p.167~168℃; I-3: white solid ( 0.56 g, 28.83 %), m.p.129~132 ℃.
[0116] The compound structure and spectrum analysis are as follows:
[0117] I-1 : 5-[4-(p-Chlorobenzyloxy)benzylidene]imidazolidine-2,4-dione
[0118] Spectrum analysis:
[0119] 1 H-NMR (DMSO-d6, 400Hz), δ : 10.654(s, 1H, N 3 H); 9.895(s, 1H, N 1 H); 7.499(s, 2H, J =8.8Hz, Ar-H); 7.381-7.415(m, 2H, Ar-H); 7.303(d, 2H, J =8.4Hz, Ar-H); 6.786(d, 2H, J =8.8...
Embodiment 3-28
[0125] With reference to the operation of Example 2, the difference is that the product of Example 1 is replaced with a halogenated compound of different structure to obtain the compound of the following general formula I
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[0128]
[0129] The measurement results of the hydrogen spectra and mass spectra of the above compounds are described below.
[0130] I-4: 5-(4-(phenylpropoxy)benzylidene)imidazolidine-2,4-dione
[0131] Spectrum analysis: 1 H-NMR (DMSO-d 6 , 400Hz), δ:10.519(s, 1H, N 3 H); 9.864(s, 1H, N 1 H); 7.485(d, 2H, J =8.4Hz, Ar-H); 7.143-7.284(m, 5H, Ar-H); 6.773(t, 2H, J =7.2Hz, Ar-H); 6.453(s, 1H, =CH); 3.486(t, 2H, J =7.2Hz, OCH 2 ); 2.586(t, 2H, J =7.2Hz, PhCH 2 ); 1.823-1.896(m, 2H, PhCH 2 CH 2 ). MS (m / z): 323.3 (M+1).
[0132] I-5: 1-phenylpropyl-5-(4-(phenylpropoxy)benzylidene)imidazolidine-2,4-dione
[0133] Spectrum analysis: 1 H-NMR (DMSO-d 6 , 400Hz), δ :10.422(s, 1H, NH); 7.635(d, 2H, J =8.6Hz, Ar-H); 7.40...
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