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Preparation method for 1-phenyl-5-mercaptotetrazole

A technology of mercaptotetrazolium and phenyl, which is applied in the field of preparation of 1-phenyl-5-mercaptotetrazolium, can solve the problems of complex operation, many types of reagents, and many reaction steps, and achieve simple operation and low production cost Low, little environmental pollution effect

Active Publication Date: 2018-12-07
ZHEJIANG BULK CHEM
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Problems solved by technology

[0003] The method for preparing PMT in the prior art is mainly to react phenyl isothiocyanate with hydrazine hydrate to generate 1-phenyl-2 thiosemicarbazide, which is cyclized by nitrous acid, and then rearranged with sodium carbonate to synthesize PMT (Synthesis of 1-substituted phenyl-5-mercaptotetrazolium, Fan Rulin et al., "Photosensitive Materials" 1984, No. 01); but this method requires many kinds of reagents, and there are many reaction steps and complicated operations

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  • Preparation method for 1-phenyl-5-mercaptotetrazole

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preparation example Construction

[0020] The invention provides a preparation method of 1-phenyl-5-mercaptotetrazolium, comprising the following steps:

[0021] Under the condition of 90~95 ℃, the sodium azide aqueous solution is mixed with phenyl isothiocyanate and then kept for 110~130min to carry out the azide reaction to obtain the azide reaction product feed liquid;

[0022] The azide reaction product feed liquid is mixed with water, the pH value of the obtained material is adjusted with hydrochloric acid to be 3.0-5.0, and acidified for 50-70 min to obtain 1-phenyl-5-mercaptotetrazolium.

[0023] In the present invention, under the condition of 90-95 DEG C, the sodium azide aqueous solution is mixed with phenyl isothiocyanate, and then the azide reaction is carried out for 110-130 min under heat preservation to obtain the azide reaction product feed liquid. In the present invention, the mass content of sodium azide in the sodium azide aqueous solution is preferably 8-12%, more preferably 9-10%. In the p...

Embodiment 1

[0042] Mix 10.0kg of purified water with 1.0kg of sodium azide to obtain an aqueous solution of sodium azide, heat it to 90°C, add 2.0kg of phenyl isothiocyanate dropwise under stirring conditions, after the dropwise addition, keep warm for 2 hours , add 0.1kg of activated carbon to the obtained system, continue to stir for 30min, remove the activated carbon by filtration, and obtain the azidation reaction product liquid;

[0043] The azidation reaction product liquid was mixed with 3 kg of purified water, and 1.5 kg of hydrochloric acid with a mass concentration of 31% was added dropwise under stirring conditions, so that the pH value of the obtained material was 4.8, and acidification treatment was carried out at 26°C for 60 minutes; The obtained system was centrifuged, and the obtained crude product was washed with 2 kg of purified water, centrifuged, and the obtained solid material was dried under reduced pressure to obtain 2.4 kg of finished 1-phenyl-5-mercaptotetrazole wi...

Embodiment 2

[0045] Mix 10.0kg of purified water with 1.0kg of sodium azide to obtain an aqueous solution of sodium azide, heat it to 95°C, add 2.05kg of phenyl isothiocyanate dropwise under stirring conditions, after the dropwise addition, keep warm for 2 hours , add 0.1kg of activated carbon to the obtained system, continue to stir for 30min, remove the activated carbon by filtration, and obtain the azidation reaction product liquid;

[0046] The azidation reaction product liquid was mixed with 3 kg of purified water, and 1.5 kg of hydrochloric acid with a mass concentration of 31% was added dropwise under stirring conditions, so that the pH value of the obtained material was 3.5, and the acidification treatment was carried out at 30° C. for 60 minutes; The obtained system was centrifuged, the obtained crude product was washed with 2 kg of purified water, centrifuged, and the obtained solid material was dried under reduced pressure to obtain 2.452 kg of 1-phenyl-5-mercaptotetrazolium fini...

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Abstract

The invention provides a preparation method for 1-phenyl-5-mercaptotetrazole. The preparation method takes sodium azide and phenyl isothiocyanate as a reaction raw material of preparing 1-phenyl-5-mercaptotetrazole by controlling a reaction temperature to 90-95 DEG C and reaction time to 110-130 min, so that full azido reaction of the sodium azide and phenyl isothiocyanate can be guaranteed undermilder conditions and without the use of a catalyst. The preparation method is simple in operation and small in environment pollution during production, and the use of complex production equipment isnot needed; and the preparation method is simple in post-treatment operation, low in production cost so that to realize large-scale industrial production is easy. Results of embodiments show that theyield of the target object (1-phenyl-5-mercaptotetrazole) can reach to 94.8% when the method is adopted to perform large-scale industrial production, so that actual production needs can be met.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 1-phenyl-5-mercaptotetrazolium. Background technique [0002] Statins are hydroxymethylglutaryl coenzyme A (HMG-CoA) reductase inhibitors. In addition to regulating blood lipids, they also have important non-oxidative, anti-inflammatory, regulating vascular endothelial function, and inhibiting thrombosis. Lipid-lowering regulation function. Among them, an important intermediate used in the preparation of statins is 1-phenyl-5-mercaptotetrazolium (PMT). In addition, PMT can also be used in photographic anti-fogging agents, electroplating additives and photosensitive material stabilizers. [0003] The method for preparing PMT in the prior art is mainly to react with phenyl isothiocyanate and hydrazine hydrate to generate 1-phenyl-2 thiosemicarbazide, which is cyclized by the action of nitrous acid, and then rearranged to synthesize PMT by the act...

Claims

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Application Information

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IPC IPC(8): C07D257/04
CPCC07D257/04
Inventor 柴寿根周峰傅桂萍陈江平
Owner ZHEJIANG BULK CHEM
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