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HRID 75446作成日:2026年10月25日

Diethyl Malonate → HCID 178526553、化合物

https://huagongshe.com/reaction/75446

反応式

関与物質

役割名称HCID仕込み量
反応物Diethyl MalonateHCID 7761—
反応物4-NitrobenzamidineHCID 117475—
反応物Sodium MethoxideHCID 10942334—
溶媒MethanolHCID 887—
生成物HCID 178526553HCID 17852655381.4%

反応手順

In a 50 mL round-bottomed flask was placed 4-nitrobenzimidamide (55, 0.435 g, 2.63 mmol) in MeOH (4 mL) to give a yellow suspension. Sodium methanolate (25% by wt in MeOH) (1.867 mL, 8.17 mmol) was added. The mixture was stirred at room temperature for 30 min. Diethyl malonate (0.480 mL, 3.16 mmol) was added in drops and stirring was continued at room temperature over 6 days, resulting in an orange suspension. The mixture was concentrated, dissolved in hot water and filtered. The filtrate was made acidic with AcOH to pH3. The resulting light yellow solids were collected by filtration and dried under vacuum to give the title compound (499 mg, 81%) as a light yellow solid. HRMS: For [M+H]+ mass error=−0.0 mDa or −0.17 ppm.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08835429B2
出典データセットuspto-grants-2014_09
ORD IDord-34ea74092a464bd39b298f2557d27d62
出典メモuspto-grants-2014_09