化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 1-(4-nitrophenyloxycarbonyl)-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 | 4-Nitrophenyl chloroformate | HCID 82129 | — |
| 反応物 | 1,2,5,6-Tetrahydropyridine-3-carboxaldehyde-O-methyloxime | HCID 197313 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-nitrophenyloxycarbonyl)-1,2,5,6-tetrahydropyridine-3-carboxaldehyde-O-methyloxime | HCID 3072863 | 95% |
反応手順
A solution of 97% 4-nitrophenyl chloroformate (1.5 g, 7.22 mmoles) in dichloromethane (15 mL) was added at 0° C. to a stirred solution of 1,2,5,6-tetrahydropyridine-3-carboxaldehyde-O-methyloxime (0.92 g, 6.6 mmoles) and triethylamine (0.92 mL, 6.6 mmoles) in dichloromethane (20 mL). The reaction mixture was then stirred at room temperature for 20 minutes, the solvent was evaporated and the residue was partitioned between water and ethyl acetate. The organic layer was dried (Na2SO4) and evaporated. The solid was recrystallized from benzene-cyclohexane to give 1.9 g (95%) of the desired product with mp 109°-110° 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-fd4c77fa32594158be7a2ba968f393e8 |
| 出典メモ | uspto-grants-1993_07 |