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HRID 351562作成日:2026年10月27日

Hydrochloric Acid → (+/-)-alpha-(3,4-Dichlorophenyl)-2,6-dimethyl-4-nitrobenzeneacetonitrile

https://huagongshe.com/reaction/351562

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Sodium hydrideHCID 24758—
反応物(3,4-Dichlorophenyl)acetonitrileHCID 76690—
反応物2-Methoxy-1,3-dimethyl-5-nitrobenzeneHCID 139835—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物(+/-)-alpha-(3,4-Dichlorophenyl)-2,6-dimethyl-4-nitrobenzeneacetonitrileHCID 2231292687%

反応条件

温度0 °C

反応手順

A mixture of (3,4-dichlorophenyl)acetonitrile (0.149 mol) in DMF (100 ml) was stirred at 0° C. under N2 flow. Sodium hydride (0.223 mol) was added portionwise. The mixture was stirred at 0° C. under N2 flow for 1 hour. A mixture of, 2-methoxy-1,3-dimethyl-5-nitrobenzene (0.149 mol) in DMF (100 ml) was added dropwise at 0° C. under N2 flow. The mixture was stirred at RT for 6 hours, then cooled, hydrolized with H2O and with HCl 3N and extracted with EtOAc. The organic layer was separated, washed several times with H2O, dried, filtered and the solvent was evaporated. The residue was crystallized from DIPE. The precipitate was filtered off and dried, yielding 43.4 g (87%) of (±)-α-(3,4-dichlorophenyl)-2,6-dimethyl-4-nitrobenzeneacetonitrile (interm. 48).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06743792B2
出典データセットuspto-grants-2004_06
ORD IDord-e22c4e17d82f4d52a1b42abd2bf3c54c
出典メモuspto-grants-2004_06