(E)-3-[2-(Pyridin-2-yl)ethenyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-6-amine synthesis
- Product Name:(E)-3-[2-(Pyridin-2-yl)ethenyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-6-amine
- CAS Number:886230-76-8
- Molecular formula:C19H20N4O
- Molecular Weight:320.39
886230-75-7
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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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