Preparation method of fluorenocarbazole organic electroluminescent material intermediate
A technology of fluorene carbazoles and intermediates, which is applied in the field of electroluminescent material synthesis, can solve the problems of poor route selectivity, difficult separation, low yield and the like, achieves high yield, high reaction selectivity and simple preparation process Effect
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[0033] The object of the present invention is to provide a kind of preparation method of fluoren and carbazole organic electroluminescence material intermediate, described method may comprise the following steps:
[0034] (1) performing acetylation protection on the starting compound containing the amino group to obtain the first intermediate;
[0035] (2) Nitrate the acetylation-protected first intermediate obtained in step (1) to obtain a second intermediate;
[0036] (3) Carry out deamination protection to the second intermediate obtained in step (2), obtain the third intermediate;
[0037] (4) converting the amino group of the third intermediate into a halogen substituent to obtain the fourth intermediate;
[0038] (5) Suzuki coupling reaction is carried out to the third intermediate obtained in step (4), to obtain the fifth intermediate whose ring-forming functional group is fixed; and
[0039] (6) cyclizing the fifth intermediate to obtain a fluorenocarbazole organic e...
Embodiment 1
[0044] This example involves the use of 2-amino-9,9-dimethylfluorene to synthesize
[0045]
[0046] The synthetic route of this embodiment is as figure 1 as shown, figure 1 The numbers below each compound in , indicate the yield. refer to figure 1 , the synthetic route of this example includes the following steps.
[0047] 1. Add 2-amino-9,9-dimethylfluorene (SM, 313.9g, 1500mmol) into a 3L four-necked flask, then add acetic acid (1150mL, 1207.5g) to dissolve, and stir evenly with a mechanical stirrer. Acetic anhydride (285 mL, 307.8 g, 3015 mmol) was slowly added dropwise (3.3 h) through a constant pressure dropping funnel with stirring at room temperature (around 25°C). Continue to stir at room temperature (about 25°C) after the dropwise addition, during which a large amount of white precipitates precipitate out, and the reaction time is about 24h (6h, central control 1; 24h central control 2). The reaction solution was poured into 5 L of water, and mechanically sti...
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