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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

反応式

関与物質

役割名称HCID仕込み量
反応物TolueneHCID 1140—
反応物Sodium hydrideHCID 24758—
反応物1,4-Dihydro-2,6-dimethyl-4-(2-(trifluoromethyl)phenyl)-3,5-pyridinedicarboxylic acid diethyl esterHCID 168089—
反応物2-chloro-N,N-bis(methoxyethyl)ethylamineHCID 15659571—
溶媒DimethylformamideHCID 6228—
生成物Diethyl 1,4-dihydro-4-(2-trifluoromethylphenyl)-2,6-dimethyl-1-(2-[N,N-bis-(methoxyethyl)]aminoethyl)-3,5-pyridine dicarboxylateHCID 20281063—

反応条件

温度50 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US04520131
出典データセットuspto-grants-1985_05
ORD IDord-19e44a28db16498895aff6545ae620b0
出典メモuspto-grants-1985_05