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A synthesis method and technology of Boldenone, applied in the directions of steroids, organic chemistry, etc., can solve the problems of many by-products, low quality, low yield, etc., and achieve improved yield and quality, strong reaction selectivity, and economical cost effect
Inactive Publication Date: 2013-04-10
YICHENG GOTO PHARMA
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Problems solved by technology
The traditional Boldenone production process uses 4-AD as a raw material, reduces it with potassium borohydride, oxidizes it with manganese dioxide, and dehydrogenates it. This route has many by-products, low quality and low yield.
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Embodiment 1
[0024] 1. Etherification reaction:
[0025] In a 300L reactor equipped with stirring, 72 kg of absolute ethanol and 42 kg of triethyl orthoformate were metered in, and then 75 kg of 1.4-ADD was added while stirring, and stirred for 5 minutes.
[0026] Adjust the temperature in the reactor to 39-42°C, then add 0.3 kg of pyridinium hydrobromide, start the reaction, record the time for 8 hours, add 1.0 Kg of triethylamine after the reaction, cool down to 0-5°C, and control the temperature at 0~5℃, keep stirring for 1 hour. When the reaction solution reaches neutrality, the etherification reaction is over, open the frozen brine, and freeze and crystallize at 0±2°C.
[0027] After the etherification reaction was terminated, the etherified compound was released from the reaction kettle, washed with 100 kg of absolute ethanol, and filtered by rejection to obtain a wet etherified compound.
[0028] 2. Reductive hydrolysis reaction:
[0029] In a 1000L washed and dried reaction pot,...
Embodiment 2
[0033] 1. Etherification reaction:
[0034] In a 300L reactor equipped with stirring, 75 kg of absolute ethanol and 45 kg of triethyl orthoformate were metered in, and then 76 kg of 1.4-ADD was added while stirring, and stirred for 5 minutes. Adjust the temperature in the reactor to 39-42°C, then add 0.2 kg of pyridinium hydrobromide, start the reaction, record the time for 8 hours, add 1.2 Kg of triethylamine after the reaction, cool down to 0-5°C, and control the temperature at 0~5℃, keep stirring for 1 hour. When the reaction solution reaches neutrality, the etherification reaction is over, open the frozen brine, and freeze and crystallize at 0±2°C.
[0035] After the etherification reaction was terminated, the etherified compound was released from the reactor, washed with 90 kg of absolute ethanol for a while, and filtered by rejection to obtain a wet etherified compound.
[0036] 2. Reductive hydrolysis reaction:
[0037] In a 1000L washed and dried reaction pot, put 6...
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Abstract
The invention relates to a high-yield Boldenone synthesis method. The method comprises the following steps of: 1, etherification reaction: adding absolute ethyl alcohol and triethyl orthoformate in a reaction kettle, stirring, adding 1.4-ADD, pyridine hydrobromide and triethylamine, freezing for crystallization, washing with absolute ethyl alcohol, and filtering in a swinging manner to get the wet etherate; 2, reduction and hydrolysis reaction: firstly, adding methyl alcohol in the reaction kettle, stirring, then, adding etherate pyridine and sodium borohydride, preserving heat for reaction, and carrying out thin layer chromatography, after the reduction reaction, regulating the temperature, regulating pH, concentrating the mixture to be in dense slurry form, adding water, cooling, centrifuging to get reduced hydrolysate, namely a Boldenone crude product, and drying; and 3, refining of crude product: adding the Boldenone crude product, methyl alcohol and water in the production kettle, heating with steam, cooling, and centrifuging. In the method, a new catalyst, namely pyridine hydrobromide, is used, thus, the yield and the quality of the product are improved. The method realizes one-step preparation of Boldenone, and in comparison with the DDQ (dihydro dicyan benzoquinone) dehydrogenation used in the past, the cost of products is saved in the synthesis method.
Description
technical field [0001] The invention relates to a method for synthesizing boldenone, in particular to a method for synthesizing high-yield boldenone. Background technique [0002] Boldenone is a derivative of testosterone and thus inherits most of the properties of testosterone, such as androgenic capacity and protein synthesis capacity. Boldenone keeps the nitrogen balance of muscle fiber cells tending to be positive at any time, accelerates the synthesis of protein by muscle fiber cells, and expands muscle fiber cells as a result, which is very effective in strengthening muscles and enhancing endurance for physical exercisers. Because Boldenone has no obvious male and female tendencies, it rarely has side effects, so it is recognized by consumers. The traditional Boldenone production process uses 4-AD as a raw material, reduces it with potassium borohydride, oxidizes it with manganese dioxide, and dehydrogenates it. This route has many by-products, low quality and low yie...
Claims
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