Preparation method of 1,3,6-hexanetricarbonitrile
A technology of hexane trinitrile and dinitrile, which is applied in the field of compound preparation, can solve the problems of poor whiteness and low purity, and achieve the effects of high yield, high product purity and easy availability of raw materials
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Embodiment 1
[0020] The preparation method of 1,3,6-hexane trinitrile includes the following steps:
[0021] A. Preparation of 1,6-Dicyano-2-butene: Using 1,4-dioxane as the reaction solvent, place 1mol1,6-dichloro-2-butene, 0.5gCuCl and 2molNaCN in 1 In ,4-dioxane, the substitution reaction is carried out at 40°C for 2h to obtain 1,6-dianitrile-2-butene;
[0022] B. Preparation of 1,3,6-hexane trinitrile: The 1,6-dianitrile-2-butene prepared in step A was reacted with 90g HCl methanol solution at 40℃ for 4h, and then NaCN was added to it at 40℃. The substitution reaction was carried out at ℃ for 2h to obtain 1,3,6-hexanetrinitrile. The calculated yield was 52.1%. The purity of the tested product was 99.55%, the product color number APHA was 15, and the product moisture was 16PPM.
Embodiment 2
[0024] The preparation method of 1,3,6-hexane trinitrile includes the following steps:
[0025] A. Preparation of 1,6-dicyano-2-butene: using 1,4-dioxane as the reaction solvent, 1mol 1,6-dichloro-2-butene, 0.5gCu 2 O and 2.5mol NaCN were placed in 1,4-dioxane, and the substitution reaction was carried out at 80°C for 5h to obtain 1,6-dianitrile-2-butene;
[0026] B. Preparation of 1,3,6-hexane trinitrile: react the 1,6-dianitrile-2-butene prepared in step A with 90g HCl methanol solution at 50℃ for 5h, and then add NaCN to 80 The substitution reaction was carried out at ℃ for 5 hours to obtain 1,3,6-hexanetrinitrile. The calculated yield was 61.2%. The purity of the tested product was 99.63%, the product color number APHA was 13, and the product moisture was 18PPM.
Embodiment 3
[0028] The preparation method of 1,3,6-hexane trinitrile includes the following steps:
[0029] A. Preparation of 1,6-Dicyano-2-butene: Using 1,4-dioxane as the reaction solvent, place 1mol1,6-dichloro-2-butene, 0.5gCuBr and 2.3molNaCN in In 1,4-dioxane, the substitution reaction was carried out at 101°C for 7 hours to obtain 1,6-dianitrile-2-butene;
[0030] B. Preparation of 1,3,6-hexane trinitrile: The 1,6-dianitrile-2-butene prepared in step A was reacted with 90g HCl methanol solution at 60°C for 6h, and then NaCN was added to it at 101 The substitution reaction was carried out at ℃ for 7 hours to obtain 1,3,6-hexanetrinitrile. The calculated yield was 57.5%. The purity of the tested product was 99.54%, the product color number APHA was 17, and the product moisture was 16PPM.
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