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Methyl iodide → O5-tert-butyl O2-ethyl 1-methyl-6,7-dihydro-4H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5-Tert-butyl 2-ethyl 6,7-dihydro-1H-pyrrolo[3,2-C]pyridine-2,5(4H)-dicarboxylate | HCID 66864309 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | O5-tert-butyl O2-ethyl 1-methyl-6,7-dihydro-4H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate | HCID 66864160 | — |
反応手順
To a solution of 5-tert-butyl 2-ethyl 1,4,6,7-tetrahydro-5H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate (1.0 eq) in THF at 0° C. was added NaH (1.2 eq) and stirred for half an hour at room temperature. Methyl iodide (1.3 eq) was added and resulting reaction mixture was stirred for 3 hrs. Reaction mixture was then quenched with water and extracted with ethyl acetate, dried over sodium sulphate and concentrated to dryness. Crude mass was then purified by silica gel column chromatography to afford 5-tert-butyl 2-ethyl 1-methyl-1,4,6,7-tetrahydro-5H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08440830B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-bd144e7436764823bf42c0c4d1686669 |
| 出典メモ | uspto-grants-2013_05 |