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ChemicalBook CAS DataBase List (E)-3-[2-(Pyridin-2-yl)ethenyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-6-amine
886230-76-8

(E)-3-[2-(Pyridin-2-yl)ethenyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-6-amine synthesis

8synthesis methods
886230-75-7 Synthesis
(E)-6-Nitro-3-[2-(pyridin-2-yl)ethenyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole

886230-75-7
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(E)-3-[2-(Pyridin-2-yl)ethenyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-6-amine

886230-76-8
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Yield: 94.38%

Reaction Conditions:

with sodiumsulfide nonahydrate in methanol at 65; for 3 h;Temperature;

Steps:

5 Example 5
35 g of II was dissolved in 350 ml of methanol and Na2S·9H2O solution was added(72 g of Na 2 S·9H 2 O/240 ml of water), and the mixture was stirred at 65° C. for 3 hours.The insoluble material was removed by suction filtration and 810 ml of water at 50° C. was added to the filtrate. The mixture was stirred at 0° C. for 2 h and filtered by suction. The filter cake was washed with methanol:water (V:V)=1:3 50 ml of solution and dried in vacuum at 40° C. 30.2 g of solid was obtained. Yield 94.38%, HPLC purity 99.2%.

References:

Lunan Pharmaceutical Group Co., Ltd.;Zhang Guimin;Liu Jianshe;Yu Junhou CN107778299, 2018, A Location in patent:Paragraph 0021-0024; 0025-0028; 0029-0030

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