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HRID 844428作成日:2026年10月27日

Hydrochloric Acid → 1-Isopropenyl-2,4-dimethoxybenzene

https://huagongshe.com/reaction/844428

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物TetrahydrofuranHCID 8028—
反応物1-(2,4-Dimethoxyphenyl)ethanoneHCID 70016—
反応物HCID 178418348HCID 178418348—
溶媒Diethyl EtherHCID 3283—
生成物1-Isopropenyl-2,4-dimethoxybenzeneHCID 10909234—

反応条件

温度0 °C

反応手順

10.57 g of 1-(2,4-dimethoxyphenyl)ethanone are dissolved in 100 ml of ether and 50 ml of THF under nitrogen. 55 ml of 1.6M methyllithium in ether are added at −50° C. and the mixture is left stirring for 2 hours between −60° C. and −40° C. and then for 30 minutes between −40° C. and 0° C. and for 3 hours at RT. It is cooled to 0° C. and 70 ml of 2N HCl are added. After separation of the phases by settling, the aqueous phase is extracted with ether and the organic phase is then dried over Na2SO4. This solution is concentrated and the residue is then taken up in 150 ml of THF and 75 ml of 2N HCl are added. After stirring for 4 hours at RT, 100 ml of water are added and this mixture is then extracted with ether. The organic phase is washed with Na2CO3, with water and then dried over Na2SO4 and concentrated. The residue is chromatographed on silica, eluting with a DCM/pentane mixture (70/30 and then 60/40). 5 g of the expected compound are obtained in the form of an oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06380230B1
出典データセットuspto-grants-2002_04
ORD IDord-dea23ab0f05b45c381c98dbd3a82f019
出典メモuspto-grants-2002_04