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HRID 1353031作成日:2026年10月26日

Sodium hydride → 9,9-Bis(N-carbazolyl-decyl)-2,7-dibromofluorene

https://huagongshe.com/reaction/1353031

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium hydrideHCID 24758—
反応物2,7-DibromofluoreneHCID 140073—
反応物9-(10-Bromodecyl)-9H-carbazoleHCID 21976310—
溶媒TetrahydrofuranHCID 8028—
生成物9,9-Bis(N-carbazolyl-decyl)-2,7-dibromofluoreneHCID 2104412834.1%

反応手順

To a mixture of 5.2 g (16 mmol) 2,7-dibromofluorene in 300 mL THF was added 1.3 g (41 mmol) sodium hydride (75%) in several portions. A mixture of 15 g (39 mol) N-(10-bromodecyl)-carbazole (8) in 100 mL THF was added dropwisely at 70° C. and the mixture was refluxed for 48 h. After cooling, the solid was filtered and the filtrate was concentrated and dilute with water and extracted with CH2Cl2. The organic layer was collected and washed with brine and dried with anhydrous MgSO4. The crude product was further purified by silica column chromography to give 5.1 g (yield 34%, mp 94˜96° C.) title product. 1H NMR (CDCl3), δ (ppm): 8.10 (4H, d), 7.38˜7.48 (14 H, m), 7.23 (4H, t), 4.27 (4H, t), 0.88˜1.86 (36H, m). Anal. Calcd: C, 73.22; H, 6.68; N, 3.00. Found: C, 72.58; H, 6.59; N, 2.73.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07220819B2
出典データセットuspto-grants-2007_05
ORD IDord-2d60f307539c4c0c9c21aec458cb0ea1
出典メモuspto-grants-2007_05