Acetylacetone copper (II) catalytic synthesis method for 1,2,3 triazole chemical compounds
A technology of copper acetylacetonate and azide compounds, which is applied in the field of synthesis of 1,2,3-triazole compounds, can solve the problems of difficult preparation of metal catalysts, tedious multi-step synthesis, and difficulty in recycling, and achieve cheap catalysts , environmental friendliness and short response time
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Embodiment 1
[0020] 10g (0.041mol) Cu(NO 3 ) 2 ·3H 2 O was dissolved in 100mL of water, and 15mL of concentrated ammonia water was added to obtain copper ammonia complex ion [Cu(NH 3 ) 4 ] 2+ Add 11 mL of acetylacetone under stirring to obtain a blue precipitate, filter and wash with water, and dry in vacuo to obtain 10.05 g of a blue powdery crude product. The crude product is refluxed and dissolved with a mixed solution of 75 mL of chloroform and 225 mL of methanol, cooled, crystallized and dried to obtain 7.48 g blue crystal copper (II) acetylacetonate for later use.
Embodiment 2
[0022] Using the copper (II) acetylacetonate obtained in Example 1 as the catalyst, add 0.0065 g (0.025 mmol) of the catalyst copper (II) acetylacetonate, 0.066 g (0.5 mmol) of phenoxypropyne, phenyl azide 0.060g (0.5mmol) and 2mL of water were stirred and reacted in an oil bath at 50°C, and the reaction process was monitored by TLC. TLC monitors that the reaction is complete in 0.5h, adding ethyl acetate for extraction, filtering the aqueous phase and the organic phase at the same time, washing the filter cake with ethyl acetate, the filter cake is blue, and there is no significant change before and after the catalyst reaction, the filtrate is separated, and organic Phase sampling was done to analyze the product by HPLC. The influence of different solvents on the reaction is shown in Table 1.
[0023] Table 1 The influence of different solvents on the reaction
[0024] .
Embodiment 3
[0026]The copper (II) acetylacetonate regenerated in Example 2 was used as the catalyst, and 0.026 g (0.1 mmol) of the recovered catalyst copper (II) acetylacetonate, 0.066 g (0.5 mmol) of phenoxypropyne, phenyl Azide 0.071g (0.6mmol) and water 2mL were stirred and reacted in an oil bath at 50°C, and the reaction process was monitored by TLC. TLC monitors that the reaction is complete after 0.5h, add ethyl acetate for extraction, filter the water phase and the organic phase simultaneously, wash the filter cake (catalyst) with ethyl acetate, separate the filtrate, take a sample of the organic phase for HPLC analysis of the product, and repeat the recovery The effect of the number of times on the reaction yield is shown in Table 2.
[0027] Table 2 The effect of the number of repetitions on the reaction yield
[0028] .
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