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Triethylamine → 1-(4-methylphenyloxycarbonyl)-1,2,5,6-tetrahydropyridine-3-carboxaldehyde-O-methyloxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | p-Tolyl chloroformate | HCID 70304 | — |
| 反応物 | 1,2,5,6-Tetrahydropyridine-3-carboxaldehyde-O-methyloxime | HCID 197313 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-methylphenyloxycarbonyl)-1,2,5,6-tetrahydropyridine-3-carboxaldehyde-O-methyloxime | HCID 3072864 | 91% |
反応手順
A solution of p-tolylchloroformate (1.5 mL, 10.3 mmoles) in dichloromethane (15 mL) was added under nitrogen at 0° C. to a stirred solution of 1,2,5,6-tetrahydropyridine-3-carboxaldehyde-O-methyloxime (1.3 g, 9.3 mmoles) and triethylamine (1.3 mL, 2.3 mmoles) in dichloromethane (20 mL). The reaction mixture was stirred at room temperature for 20 minutes, the solvent was evaporated and the residue was partitioned between water and ethylacetate. The organic layer was dried (Na2SO4) and evaporated. The solid was triturated with cyclohexane to afford 2.3 g (91%) of a white solid with mp 70°-71° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05231107 |
| 出典データセット | uspto-grants-1993_07 |
| ORD ID | ord-9de783cbaa2b4fa6addc4ca21f17934b |
| 出典メモ | uspto-grants-1993_07 |