Preparation method of 2-amino-9, 9-diphenylfluorene
A technology of diphenylfluorene and amino, which is applied in the field of liquid crystal compound synthesis, can solve the problems of unfavorable mass production and high production cost, and achieve the effects of reduced production cost, high product yield and simple process flow
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[0033] The invention provides a preparation method of 2-amino-9,9-diphenylfluorene, which comprises the following steps.
[0034] A) using 9-fluorenone as a raw material, through a bromination reaction, to obtain 2-bromo-9-fluorenone, the structural formula is,
[0035] The specific preparation method of 2-bromo-9-fluorenone is as follows.
[0036] A1) Add 9-fluorenone, acetic acid, water, and concentrated sulfuric acid in sequence in a three-necked flask, and mix well to obtain a reaction solution a1. The structural formula of 9-fluorenone is:
[0037] A2) The temperature of the reaction solution a1 is raised to 50-60 degrees Celsius, after slowly adding liquid bromine dropwise, it is incubated for 5-8 hours, and cooled to room temperature to obtain the reaction solution a2; wherein, the molar ratio of 9-fluorenone to liquid bromine is 1: 1~1.5.
[0038] A3) Suction filtration of the reaction solution a2 to obtain a filter cake. After washing the filter cake, vacuum-dry...
Embodiment 1
[0055] This embodiment is used to prepare the preparation method of 2-amino-9,9-diphenylfluorene, which specifically includes the following steps.
[0056] A) with 9-fluorenone As a raw material, 2-bromo-9-fluorenone is obtained by bromination reaction,
[0057] A1) There is a three-necked flask equipped with a stirring, thermometer, and constant pressure dropping funnel. Add 9-fluorenone (5.4g, 30mmol), 33mL of acetic acid, 11mL of water, and 0.8g of concentrated sulfuric acid into the three-necked flask, mix them, and stir evenly to obtain the reaction solution a1 .
[0058] A2) Reaction solution a1 was warmed up to 51 degrees centigrade, and liquid bromine (4.8 g, 39 mmol) was slowly added dropwise. After addition, the temperature was raised to 58 degrees centigrade, kept for 6 hours, and cooled to room temperature to obtain reaction solution a2.
[0059] A3) The reaction solution a2 is suction filtered, and the filter cake is washed 3 times with acetic acid-water solu...
Embodiment 2
[0075] This embodiment is used to prepare the preparation method of 2-amino-9,9-diphenylfluorene, which specifically includes the following steps.
[0076] A) using 9-fluorenone as a raw material, through a bromination reaction to obtain 2-bromo-9-fluorenone,
[0077] A1) There is a three-necked flask equipped with a stirring, thermometer, and constant pressure dropping funnel, to which 9-fluorenone (6.8g, 38mmol), 35mL of acetic acid, 15mL of water, and 0.96g of concentrated sulfuric acid are added and mixed, and stirred evenly to obtain the reaction solution a1 .
[0078] A2) Reaction solution a1 was warmed up to 51 degrees Celsius, and liquid bromine (5.6 g, 40 mmol) was slowly added dropwise. After the addition, the temperature was raised to 58 degrees Celsius, kept for 8 hours, and cooled to room temperature to obtain reaction solution a2.
[0079] A3) The reaction solution a2 is suction filtered, and the filter cake is washed 3 times with acetic acid-water solution wi...
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