関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-(Methanesulfonyl)-5,6-diphenyl-1,2,4-triazine | HCID 12915481 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 2-(5,6-Diphenyl-1,2,4-triazin-3-yl)acetate | HCID 12915487 | — |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728014B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-b001ef4de7204123bc89d9ca3f7063f6 |
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| 出典メモ | uspto-grants-2010_06 |
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