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HRID 12564作成日:2026年10月26日

Ethyl Acetoacetate → Ethyl 2-(5,6-Diphenyl-1,2,4-triazin-3-yl)acetate

https://huagongshe.com/reaction/12564

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl AcetoacetateHCID 8868—
反応物Sodium hydrideHCID 24758—
反応物3-(Methanesulfonyl)-5,6-diphenyl-1,2,4-triazineHCID 12915481—
溶媒TetrahydrofuranHCID 8028—
生成物Ethyl 2-(5,6-Diphenyl-1,2,4-triazin-3-yl)acetateHCID 12915487—

反応条件

温度60 °C

反応手順

To a suspension of NaH (41 mg, 1.61 mmol) in THF (2 ml) at 0° C. was added ethyl acetoacetate (105 mg. 0.80 mmol) dropwise. After the mixture was stirred for 15 min, a solution of 3-(methylsulfonyl)-5,6-diphenyl-1,2,4-triazine (Compound 87) (250 mg, 0.80 mmol) in THF (3 ml) was cannulated into the solution, and the resulting solution was heated to 60° C. for 2 hours. The reaction was then quenched with water. The product was extracted with ethyl acetate. The organic layer was washed with water, and brine, and dried over Na2SO4. The filtered solvent was concentrated in vacuo, and the residue was purified by silica gel chromatography (20% ethyl acetate in hexane) to give title compound as a solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07728014B2
出典データセットuspto-grants-2010_06
ORD IDord-b001ef4de7204123bc89d9ca3f7063f6
出典メモuspto-grants-2010_06