A kind of thiazolopyrimidinone compound and its preparation method and application
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 high selectivity, strong activity, and obvious activity-concentration dose-effect relationship Effect
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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 (Code: JWX-A0824)
[0037] 1. Synthesis of 2-chloro-N-(2-chloro-6-methylphenyl)acetamide (A2)
[0038]
[0039] Compound A1 (14.2 g, 100 mmol) was dissolved in 100 ml of acetic acid and 80 ml of saturated sodium acetate aqueous solution, and chloroacetyl chloride (17.0 g, 150 mmol) was added under ice bath, which quickly became turbid, slowly warmed to room temperature, and stirred overnight. Add 100 ml of water, filter with suction, wash with water, and dry to obtain 12.7 g of white solid, denoted as A2, with a yield of 58.0%. The crude product was not purified and was directly put into the next step.
[0040] 2. Synthesis of 4-amino-N-(2-chloro-6-methylphenyl)-2-ethylthiothiazole-5-carboxamide (A3)
[0041]
[0042] Compound A2 (10.9 g, 50 mmol) was dissolved in 100 ml of acetone, 100 ml of an aqueous solution of dipotassium cyanamide dithioformate (9.7 g, 50 mm...
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 (Code: LD486)
[0051]
[0052] Compound A5 (370 mg, 1.0 mmol) and 2-methyl-4-amino-6-chloropyrimidine b1 (287 mg, 2.0 mmol) were dissolved in 3 ml of anhydrous THF, NaH (48 mg, 2.0 mmol) was added, and drying was added to condense Tube with balloons on top. Heat to reflux for 0.5h. The reaction was stopped, cooled to room temperature, poured into ice water, and diluted hydrochloric acid was added dropwise to adjust the pH to neutrality, and a large amount of solid was precipitated. Suction filtration, washing and drying to obtain 398 mg of yellow solid with a yield of 95.0%. Recrystallization 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...
Embodiment 3
[0054] Example 3: Preparation of 6-(2-Chloro-6-methylphenyl)-2-p-methylanilinothiazolo[4,5-d]pyrimidin-7(6H)-one (Code: JWX-A1029)
[0055]
[0056] The synthetic method is the same as that of 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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