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HRID 2277358作成日:2026年10月26日

Nitrogen → [4'-(8,12b-Diazabenzo[a]aceanthrylen-8-yl)biphenyl-4-yl]diphenylamine

https://huagongshe.com/reaction/2277358

反応式

関与物質

役割名称HCID仕込み量
反応物NitrogenHCID 947—
反応物Tris(1,1-dimethylethyl)phosphineHCID 83681—
反応物4-Bromo-4'-(diphenylamino)biphenylHCID 11315550—
反応物Sodium t-butoxideHCID 23676156—
反応物8H-8,12b-Diazabenzo[a]aceanthryleneHCID 67110567—
触媒palladium(II) acetateHCID 167845—
溶媒WaterHCID 962—
溶媒1,4-DioxaneHCID 31275—
生成物[4'-(8,12b-Diazabenzo[a]aceanthrylen-8-yl)biphenyl-4-yl]diphenylamineHCID 67324186—

反応手順

A degassed solution of 35.6 g (89 mmol) of (4′-bromobiphenyl-4-yl)-diphenylamine and 22.0 g (81 mmol) of 8H-8,12b-diazabenzo[a]aceanthrylene in 1000 ml of dioxane is saturated with N2 for 1 h. Then firstly 1.0 ml (4 mmol) of P(tBu)3, then 0.4 g (2 mmol) of palladium(II) acetate are added to the solution, and 11.7 g (122 mmol) of NaOtBu in the solid state are subsequently added. The reaction mixture is heated under reflux for 18 h. After cooling to room temperature, 1000 ml of water are carefully added. The organic phase is separated off, washed with 4×50 ml of water and dried over MgSO4, and the solvent is removed in vacuo. The pure product is obtained by recrystallisation and final sublimation in a high vacuum.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09133119B2
出典データセットuspto-grants-2015_09
ORD IDord-ecf6fc362d3a484090a4aaeee18f7bf1
出典メモuspto-grants-2015_09