2012•Journal of Liaoning University of TechnologyRequires access

Synthesis of cyclohexanol

Qi Hang

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Abstract

The cycloheptanone was synthesized with the main material 1-(Nitromethyl)-cyclohemanol through iron reduction,diazotization and ring expansion reaction.The purity of samples by GC spectrum was determined and the structure was characterized by IR spectrum and H-NMR spectrum.The effects of the synthesis conditions on the yield of product were discussed,with much better synthesizing process found.The results indicate that the optimal synthesis conditions are as follows: the molar ratio of iron powder to 1-(nitromethyl)-cyclohemanol is 3.5:1.0,the control range of iron reduction PH is 5~6,the temperature of iron reduction is 40 ℃,the temperature of diazotization is below 5℃,the control range of diazotization PH is 3~4.The yield of products is 48.69%.

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What this paper is about

The cycloheptanone was synthesized with the main material 1-(Nitromethyl)-cyclohemanol through iron reduction,diazotization and ring expansion reaction.The purity of samples by GC spectrum was determined and the structure was characterized by IR spectrum and H-NMR spectrum.The effects of the synthesis conditions on the yield of product were discussed,with much better synthesizing process found.The results indicate that the optimal synthesis conditions are as follows: the molar ratio of iron powder to 1-(nitromethyl)-cyclohemanol is 3.5:1.0,the control range of iron reduction PH is 5~6,the temperature of iron reduction is 40 ℃,the temperature of diazotization is below 5℃,the control range of diazotization PH is 3~4.The yield of products is 48.69%.

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Available abstract

The cycloheptanone was synthesized with the main material 1-(Nitromethyl)-cyclohemanol through iron reduction,diazotization and ring expansion reaction.The purity of samples by GC spectrum was determined and the structure was characterized by IR spectrum and H-NMR spectrum.The effects of the synthesis conditions on the yield of product were discussed,with much better synthesizing process found.The results indicate that the optimal synthesis conditions are as follows: the molar ratio of iron powder to 1-(nitromethyl)-cyclohemanol is 3.5:1.0,the control range of iron reduction PH is 5~6,the temperature of iron reduction is 40 ℃,the temperature of diazotization is below 5℃,the control range of diazotization PH is 3~4.The yield of products is 48.69%.

Key concepts: Yield (engineering), Cyclohexanol, Chemistry, Iron powder, Molar ratio, Ring (chemistry), Reducing agent, Reaction conditions

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