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HRID 463533作成日:2026年10月24日
Toluene → Diethyl 1,4-dihydro-4-(2-trifluoromethylphenyl)-2,6-dimethyl-1-(2-[N,N-bis-(methoxyethyl)]aminoethyl)-3,5-pyridine dicarboxylate
https://huagongshe.com/ja/reaction/463533
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,4-Dihydro-2,6-dimethyl-4-(2-(trifluoromethyl)phenyl)-3,5-pyridinedicarboxylic acid diethyl ester | HCID 168089 | — |
| 反応物 | 2-chloro-N,N-bis(methoxyethyl)ethylamine | HCID 15659571 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Diethyl 1,4-dihydro-4-(2-trifluoromethylphenyl)-2,6-dimethyl-1-(2-[N,N-bis-(methoxyethyl)]aminoethyl)-3,5-pyridine dicarboxylate | HCID 20281063 | — |
反応手順
To a suspension of sodium hydride (5.2 gms.; 0.11 mole) (50% suspension mineral oil) in 100 ml of dry distilled DMF is added a solution of diethyl 1,4-dihydro-4-(2-trifluoromethylphenyl)-2,6-dimethyl-3,5-pyridine dicarboxylate (39.7 gms.; 0.1 mole) in 150 ml of DMF. After the gassing has ceased, the reaction mixture is heated on a water bath for 1 hour and then is cooled to 50° C. and to the hot solution is added a toluene solution of 2-chloro-N,N-bis(methoxyethyl)ethylamine. The reaction mixture is heated at 100°-110° C. for a period of 8 hours and then cooled. The unreacted NaH and NaCl is filtered off and the solvent removed from the filtrate. The residue is extracted with hot hexane which, on cooling, affords the desired product. Recrystallization from heptane yields the pure product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04520131 |
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| 出典データセット | uspto-grants-1985_05 |
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| ORD ID | ord-19e44a28db16498895aff6545ae620b0 |
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| 出典メモ | uspto-grants-1985_05 |
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