- Preparation method of substituted 2, 3-phthalazinone compound
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The invention provides a preparation method of a substituted 2, 3-phthalazinone compound. The method includes the steps of: (1) adding substituted hydrazine and substituted o-carboxybenzaldehyde intoa reaction container, controlling the reaction temperature at 50DEG C-150DEG C, and carrying out thermal insulation reaction under mechanical mixing; and (2) carrying out TLC or gas phase monitoring reaction, at the end of the reaction, adding a precipitating agent into the reaction system, conducting stirring for 0.5-1.0h, and conducting standing and filtering to obtain a solid crystal, i.e. thesubstituted 2, 3-phthalazinone compound. Starting from cheap and easily available raw materials, the preparation method provided by the invention employs one-pot process for efficient preparation of aseries of highly bioactive substituted 2, 3-phthalazinone compounds with a yield of 90%-99% under a molten state. The method has the characteristics of wide substrate application range, no adding ofcatalyst, no use of solvent and mild conditions, the reaction time is shortened by 95% or more than that of the catalytic preparation method under the traditional solvent condition, and the product purity is very high.
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Paragraph 0081; 0082
(2018/07/30)
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- Microwave-promoted solid-acid-catalyzed one-pot synthesis of phthalazinones
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A one-pot, solid-acid-catalyzed, microwave-assisted synthesis of phthalazinones is described. The commercially available montmorillonite K-10 effectively catalyzed the condensation and substitution reactions. The approach was based on the direct cyclization of phthalaldehydic acid and opianic acid with substituted hydrazines. The reactions provided excellent yields and high selectivities in very short time (5-35 minutes). Georg Thieme Verlag Stuttgart.
- Outerbridge, Verona M.,Landge, Shainaz M.,Tamaki, Hiroko,Toeroek, Bela
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experimental part
p. 1801 - 1806
(2009/12/29)
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