- Preparation method of PI3K inhibitor
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The invention provides a preparation method of a PI3K inhibitor. The PI3K inhibitor is (S)-2-[1-(9H-purine-6-ylamino) ethyl]-3-(dimethylamino)-5-fluoroquinazoline-4 (3H)-ketone, and the structural formula of the PI3K inhibitor is shown in the specification. The method comprises three steps of reactions. The method has the advantages of simple reaction steps, mild reaction conditions, indiscriminate application of the solvent, economy and environmental protection. The PI3K inhibitor is subjected to optical purification and salifying crystallization refining through organic acid resolution and has simplicity in operation, improved yield, low cost and more stable batch-to-batch quality in comparison with present silica gel column chromatography and preparation separation and is suitable for industrial production.
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Paragraph 0042-0047; 0054-0057
(2020/08/02)
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- Synthesis, structure, and characteristics of 1,2-dichlorovinyl alkyl ketones
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A method of alkyl 1,2-dichlorovinyl ketones preparation from acyl halides and 1,2-dichloroethylene was developed. The configurational equilibrium and electronic structure of alkyl 1,2-dichlorovinyl ketones was investigated by IR, 1H and 13C NMR spectroscopy, by measuring dipole moments, and by quantum-chemical calculations using methods RHF and B3LYP in the basis 6-311++G (d,p). Alkyl 1,2-dichlorovinyl ketones are stable in the Z, s-cis-configuration where the olefin proton is involved into an intramolecular hydrogen bond with the oxygen of the carbonyl group. Reaction of 1,2-dichlorovinyl ketones with alkylhydrazines afforded 1-alkyl-3-alkyl-4- chloropyrazoles. The reaction of alkyl 1,2-dichlorovinyl ketones with 1,1-dimethylhydrazine involved dehydrochlorination and afforded 1,1-dimethylhydrazinium hydrochloride and a mixture of compounds with uncertain structure. 2004 MAIK "Nauka/Interperiodica".
- Bozhenkov,Leckovskaya,Larina,Ushakov,Dolgushin,Mirskova
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p. 1583 - 1592
(2007/10/03)
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- Amidrazones. 14. The Formation of 1,1-Disubstituted Hydrazines from the Base-promoted Hydrolysis of 1,1-Disubstituted-3-amino-4,5-dihydro-1H-pyrazolium Halides: Mechanistic Considerations
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Three mechanistic pathways are considered for the hydroxide-promoted conversion of 1,1-disubstituted-3-amino-4,5-dihydro-1H-pyrazolium halides 1 to 1,1-disubstituted hydrazines, ammonia and sodium 3-hydroxypropanoate.Evidence presented in this paper supports a hydrolysis mechanism c that is initiated by hydroxide ion addition to the 3-position of 1 to form a tetrahedral intermediate 7.
- Smith, Richard F.,Dennis, Lisa A.,Ryan, William J.,Rodriguez, George,Brophy, Keith A.
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p. 181 - 183
(2007/10/02)
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