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Hydrochloric Acid → benzyl 2-ethyl-4-oxo-3,4-dihydropyridine-1(2H)-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | 4-Methoxypyridine | HCID 69278 | — |
| 反応物 | HCID 178418443 | HCID 178418443 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | benzyl 2-ethyl-4-oxo-3,4-dihydropyridine-1(2H)-carboxylate | HCID 53419195 | 89.9% |
反応手順
To a solution of 4-methoxylpyridine 81 (4.41 g, 40.5 mmol) in toluene (200 mL) at −20° C. was added CbzCl (5.7 ml, 40.5 mmol) in toluene (200 mL) dropwise. After 15 min, ethylmagnesium bromide (23 mL, 2M in THF, 46 mmol) was added dropwise. After 1 hr, 10% aqueous HCl (100 mL) was added and the mixture stirred overnight. The mixture was separated and the organic layer was washed with sat. NaHCO3 and brine. It was dried and concentrated to afford 82 (9 g, 36.4 mmol, 89.9%) that was used directly in the next reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732609B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-5516529a5feb4309858df49e05ee3ecc |
| 出典メモ | uspto-grants-2010_06 |