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Ethyl oxoacetate → Ethyl [(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amino]acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl oxoacetate | HCID 70211 | — |
| 反応物 | 5,7-Difluoro-1,2,3,4-tetrahydronaphthalen-2-ylamine | HCID 19699423 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl [(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amino]acetate | HCID 19699373 | 85.1% |
反応手順
A mixture of 5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-ylamine (6.0 g, 32.8 mmol), prepared as in Example 8, and ethyl glyoxylate (4.6 g, 36.0 mmol) in 300 mL of ethanol was hydrogenated over 10% palladium on carbon (0.75 g) for 10 hours. The mixture was filtered and concentrated by evaporation. Purification of the residue by column chromatography on silica gel (elution: 30% ethyl acetate/hexane) gave ethyl[(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amino]acetate (7.5 g, 27.9 mmol) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05719280 |
| 出典データセット | uspto-grants-1998_02 |
| ORD ID | ord-50e16a5b33bd4c9b8e2ac41645b2b19b |
| 出典メモ | uspto-grants-1998_02 |