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HRID 21461作成日:2026年10月27日

Carbon Dioxide → Benzoic acid, 2-(methylthio)-4-(trifluoromethyl)-

https://huagongshe.com/reaction/21461

反応式

関与物質

役割名称HCID仕込み量
反応物Carbon DioxideHCID 280—
反応物Hydrochloric AcidHCID 313—
反応物Benzene, 1-bromo-2-(methylthio)-4-(trifluoromethyl)-HCID 11000144—
反応物ButyllithiumHCID 178418339—
溶媒Diethyl EtherHCID 3283—
生成物Benzoic acid, 2-(methylthio)-4-(trifluoromethyl)-HCID 11085762—

反応手順

n-Butyllithium (2.5M in hexane, 25 ml) was added under an inert atmosphere to a stirred solution of 4-bromo-3-(methylsulphenyl)benzotrifluoride (16.4 g) in ether maintaining the temperature below -70° C. for 2 hours. The mixture was poured onto solid carbon dioxide pellets, stirred for 10 rains and aqueous hydrochloric acid added. The layers were separated and the aqueous layer was extracted with ether. The combined organic layers were washed with water, dried (MgSO4) and filtered. The filtrate was evaporated and the residue was triturated with cyclohexane and filtered to give 2-(methylsulphenyl)-4-trifluoromethylbenzoic acid (12.4 g) as a white solid NMR (CDCl3 +DMSO-d6): 2.45 (s,3H), 7.2(d,1H), 7.3(s,1H), 8.0(d,1H), 10.7-11(bs,1H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05424276
出典データセットuspto-grants-1995_06
ORD IDord-4b763ab9c11f46fdbe59706e9ea487f7
出典メモuspto-grants-1995_06