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A kind of preparation method of 1-phenyl-5-mercaptotetrazolium

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

Active Publication Date: 2020-06-09
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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  • A kind of preparation method of 1-phenyl-5-mercaptotetrazolium

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preparation example Construction

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

[0021] Under the condition of 90-95°C, mix the aqueous solution of sodium azide and phenyl isothiocyanate and keep it warm for azidation reaction for 110-130 minutes to obtain the azidation reaction product liquid;

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

[0023] In the present invention, under the condition of 90-95 DEG C, the sodium azide aqueous solution and phenyl isothiocyanate are mixed, and then kept warm for 110-130 minutes of azidation reaction to obtain the azidation reaction product 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 present invention, th...

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-toxic effects such as anti-oxidation, anti-inflammation, regulation of vascular endothelial function, and inhibition of thrombosis. Fat-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, etc. [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 sodiu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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