Preparation method of 2-thioxo-2,3-dihydroquinazoline-4(1H)-one compound
A compound and condensation reaction technology, applied in the direction of organic chemistry, etc., can solve the problems of difficult availability, low yield and high reaction temperature, and achieve the effects of mild conditions, high yield and low cost
Inactive Publication Date: 2018-11-13
LIANHE CHEM TECH +2
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Problems solved by technology
[0008] The technical problem to be solved by the present invention is to overcome the high cost of raw material reagents, difficulty in obtaining and high reaction temperature in the existing 2-thio-2,3-dihydroquinazolin-4(1H)-one compound preparation method , low yield, unsuitable for industrialized production and other defects, and a preparation method of 2-thio-2,3-dihydroquinazolin-4(1H)-one compounds is provided, the method conditions are mild, Green environmental protection, low cost, high yield, simple, efficient, suitable for industrial production
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment 1
[0033]
[0034] In a 2000ml reaction flask, drop into 900mL of n-butanol, 216g (1mol) of 2-amino-5-bromobenzoic acid, slowly add 111.3g (1.1mol) of triethylamine dropwise, control the temperaturet =8.15min, m / z 298.987(ES+)
Embodiment 2
[0036]
[0037] Put 900mL of n-butanol and 155.1g (1mol) of 2-amino-5-fluorobenzoic acid into a 2000ml reaction flask, slowly add 111.3g (1.1mol) of triethylamine dropwise, control the temperature t =8.04min, m / z239.06(ES+)
Embodiment 3
[0039]
[0040] Put 900mL of n-butanol and 171.6g (1mol) of 2-amino-5-chlorobenzoic acid into a 2000ml reaction flask, slowly add 111.3g (1.1mol) of triethylamine dropwise, control the temperature t =8.09min, m / z255.05(ES+)
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The invention discloses a preparation method of a 2-thioxo-2,3-dihydroquinazoline-4(1H)-one compound. The preparation method of the compound of formula I includes the following steps: a compound of formula II and a compound of formula III are subjected to a condensation reaction in an organic solvent under the action of an organic base to obtain the compound of the formula I, wherein the reactiontemperature is 70-155 DEG C, X1, X2, X3 and X4 are independently hydrogen or halogen, and R is hydrogen or one of alkyl groups of C1-C4. The preparation method provided by the invention is mild in conditions, environment-friendly, low in cost, high in yield, simple and efficient, and is suitable for industrial production. The formula of the reaction is shown in the description.
Description
technical field [0001] The invention relates to a preparation method of 2-thioxo-2,3-dihydroquinazolin-4(1H)-one compounds. Background technique [0002] 2-Thio-2,3-dihydroquinazolin-4(1H)-ones are important heterocyclic compounds with good biological and pharmacological activities, widely found in natural products and medicinal compounds Among them, a variety of derivatives have been developed into anticancer, antibacterial, anti-inflammatory and antihypertensive drugs. 2-thio-2,3-dihydroquinazolin-4(1H)-one compounds are not only used in medicine, but also widely used in the field of pesticides, such as the fungicide propoxyquinoline. [0003] The traditional synthesis method of 2-thio-2,3-dihydroquinazolin-4(1H)-ones is to react anthranilic acid or its derivatives with isothiocyanate, but isothiocyanate Unstable, difficult synthesis and storage process, limiting its practical application. [0004] Kumar, Arbind et al reported the reaction of anthranilic acid and N-n-bu...
Claims
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Login to View More IPC IPC(8): C07D239/95
CPCC07D239/95
Inventor 陈建国徐晓明陈宇黄超
Owner LIANHE CHEM TECH



