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HRID 498944作成日:2026年10月25日

Potassium Carbonate → HCID 178509606、化合物

https://huagongshe.com/reaction/498944

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物1,1,1-Trifluoro-2-iodoethaneHCID 67709—
反応物Sodium Formaldehyde SulfoxylateHCID 23689980—
反応物HCID 178509604HCID 178509604—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物HCID 178509606HCID 178509606142.3%

反応手順

2.7 g (5.0 mmol) of 1,1′-thiodi-[2-cyano-5-(3-trifluoromethylpyrazolyl)benzene], 3.0 g (19.5 mmol) of Rongalite, 3.0 g (21.7 mmol) of potassium carbonate and 6.1 g (29.0 mmol) of 2,2,2-trifluoroethyl iodide were stirred in 50 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 2.5 g of 2-(2,2,2-trifluoroethylthio)-4-(3-trifluoromethylpyrazolyl)benzonitrile (yield 71.4%) as a brown solid (m.p. 65-67° C.).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07767626B2
出典データセットuspto-grants-2010_08
ORD IDord-003062d3a2e549e7ac93dd195807b67a
出典メモuspto-grants-2010_08