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HRID 717990作成日:2026年10月27日

Potassium Phosphate, Tribasic → Dibenzofuran, 4-methyl-

https://huagongshe.com/reaction/717990

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium Phosphate, TribasicHCID 62657—
反応物4-IododibenzofuranHCID 458257—
反応物TrimethylboroxineHCID 574072—
触媒Bis(dibenzylideneacetone)palladiumHCID 9811564—
触媒2-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 11269872—
溶媒WaterHCID 962—
溶媒TolueneHCID 1140—
生成物Dibenzofuran, 4-methyl-HCID 43489554.3%

反応手順

4-Iododibenzo[b,d]furan (10 g, 34.0 mmol) and potassium phosphate (23.49 g, 102 mmol) were dissolved in 200 mL of toluene and 20 mL of water. The reaction was purged with nitrogen for 20 minutes and then 2,4,6-trimethyl-1,3,5,2,4,6-trioxatriborinane (5.34 mL, 5.94 mmol), Pd2(dba)3 (0.311 g, 0.34 mmol) and S-Phos (0.558 g, 1.36 mmol) were added. The reaction was refluxed for 18 hours. After allowing the reaction to cool to room temperature, 100 mL of water was added, the organic and aqueous layers were separated, and the aqueous layer extracted twice with 100 mL of toluene. The organic layers were passed through a plug of silica gel, eluting with DCM. After evaporation of the solvent, the crude product was subjected to column chromatography (SiO2, 3% ethyl acetate in hexane to 5% ethyl acetate in hexane, v/v) to yield 6 g (96.7%) pure product which was confirmed GC.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09193745B2
出典データセットuspto-grants-2015_11
ORD IDord-7cb3671deae64fd89ec0c2f9db78670f
出典メモuspto-grants-2015_11