Thiazole and pyrimidone compound and preparation method and application thereof
A technology of compound and pyrimidinone, which is applied in the field of thiazolopyrimidinone compound and its preparation, can solve the problems of lower learning and memory ability and increase learning and memory, and achieve the effect of high selectivity, strong activity and low risk of cardiotoxicity
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Embodiment 1
[0036] Example 1: Preparation of 6-(2-chloro-6-methylphenyl)-2-anilinothiazolo[4,5-d]pyrimidin-7(6H)-one (No. JWX-A0824)
[0037] 1. Synthesis of 2-chloro-N-(2-chloro-6-methylphenyl)acetamide (A2)
[0038]
[0039] Compound A1 (14.2g, 100mmol) was dissolved in 100ml of acetic acid and 80ml of saturated sodium acetate aqueous solution, and chloroacetyl chloride (17.0g, 150mmol) was added under ice-cooling, cloudiness soon appeared, slowly rose to room temperature, and stirred overnight. Add 100ml of water, filter with suction, wash with water, and dry to obtain 12.7g of white solid, denoted as A2, with a yield of 58.0%. The crude product was directly submitted to the next step without purification.
[0040] 2. Synthesis of 4-amino-N-(2-chloro-6-methylphenyl)-2-ethylthiothiazole-5-carboxamide (A3)
[0041]
[0042] Dissolve compound A2 (10.9g, 50mmol) in 100ml of acetone, add 100ml of aqueous solution of dipotassium cyanamide dithioformate (9.7g, 50mmol) into the syste...
Embodiment 2
[0050] Example 2: Preparation of 2-(6-chloro-2-methylpyrimidin-4-amino)-6-(2-chloro-6-methylphenyl)thiazolo[4,5-d]pyrimidin-7(6H)-one (No.: LD486)
[0051]
[0052] Compound A5 (370mg, 1.0mmol) and 2-methyl-4-amino-6-chloropyrimidine b1 (287mg, 2.0mmol) were dissolved in 3ml of anhydrous THF, NaH (48mg, 2.0mmol) was added, dried and condensed tube, with balloons on top. Heat to reflux for 0.5h. The reaction was stopped, cooled to room temperature, poured into ice water, and dilute hydrochloric acid was added dropwise to adjust the pH to neutral, and a large amount of solids were precipitated. Suction filtration, washing and drying gave 398 mg of yellow solid, yield 95.0%. Recrystallized from ethanol, m.p.>300°C, recorded as LD486.
[0053] 1 H-NMR (400MHz, DMSO-d 6 )δ8.44(s,1H),7.65–7.40(m,3H),6.99(s,1H),2.56(s,3H),2.15(s,3H). 13 C-NMR (101MHz, DMSO-d 6 )δ167.8, 164.0, 159.5, 158.1, 155.9, 150.9, 139.1, 134.0, 132.3, 131.4, 130.3, 128.1, 112.0, 104.6, 25.5, 18.2. ...
Embodiment 3
[0054] Example 3: Preparation of 6-(2-chloro-6-methylphenyl)-2-p-methylanilinothiazolo[4,5-d]pyrimidin-7(6H)-one (No. JWX-A1029)
[0055]
[0056] The synthesis method is the same as compound JWX-A0824. White solid, yield 88.8%, m.p. 241-246°C, denoted as JWX-A1029.
[0057] 1 H-NMR (400MHz, CDCl 3 )δ10.08(s,1H),7.81(s,1H),7.45(d,J=8.3Hz,2H),7.33(d,J=7.8Hz,1H),7.26(t,J=7.8Hz, 1H), 7.19(d, J=9.8Hz, 1H), 7.12(d, J=8.2Hz, 2H), 2.27(s, 3H), 2.13(s, 3H). 13 C-NMR (101MHz, CDCl 3 )δ171.41, 165.98, 155.47, 149.13, 138.64, 136.39, 135.17, 133.73, 132.90, 130.77, 130.08, 129.59, 128.03, 121.07, 108.21, 21.02, 18.35.
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