2-[(6-CHLORO-2,4-DIOXO-3,4-DIHYDROPYRIMIDIN-1(2H)-YL)METHYL]BENZONITRILE synthesis
- Product Name:2-[(6-CHLORO-2,4-DIOXO-3,4-DIHYDROPYRIMIDIN-1(2H)-YL)METHYL]BENZONITRILE
- CAS Number:865758-95-8
- Molecular formula:C12H8ClN3O2
- Molecular Weight:261.66
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Yield: 93.5%
Reaction Conditions:
with sodium hydride;lithium bromide in dimethyl sulfoxide;N,N-dimethyl-formamide at 20; for 12 h;
Steps:
2-3 Example 3: Preparation of intermediate compound 3 by the method of the present invention
Starting compound 1 (10.0 g, 68 mmol) was added to 100 ml of a 1:1 volume ratio of DMSO/DMF mixed solvent.Stir at room temperature.After being dissolved,Add 2.5g of sodium hydride,2.5 g of lithium bromide and 5 g of the composite oxide prepared in Example 1.The starting compound 2 (13.4 g, 68 mmol) was dissolved in 30 ml of a 1:1 volume ratio of DMSO/DMF mixed solvent.And slowly adding a solution of the compound 2 to the mixed solution of the compound 1 under stirring.The reaction was stirred for 12 h.The reaction solution was filtered and concentrated to give a crude material.After purification by silica gel column chromatography (dichloromethane/acetone, 75:25 isocratic elution), intermediate compound 3 was obtained.The intermediate compound 3 had a dry weight of 16.5 g and a yield of 93.5%.
References:
Zhang Zhengguang CN108727280, 2018, A Location in patent:Paragraph 0027-0032
22115-41-9
442 suppliers
$5.00/5g
865758-95-8
111 suppliers
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