3-Ethoxyandrosta-3,5-dien-17β-ol synthesis
- Product Name:3-Ethoxyandrosta-3,5-dien-17β-ol
- CAS Number:26614-48-2
- Molecular formula:C21H32O2
- Molecular Weight:316.48
972-46-3
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26614-48-2
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Yield:26614-48-2 84%
Reaction Conditions:
with potassium borohydride in methanol at 20 - 25;Reagent/catalyst;Solvent;
Steps:
2.B B, reduction product preparation
In a 1000 ml three-neck bottle, add 100g etherification product, 800 ml methanol, stirred and heated up to 20 - 25 °C, slowly add 12g potassium borohydride, 0.5 - 1.0 hours addition complete, and then continue to maintain temperature stir reaction for 2-3 hours, TLC detection end point of the reaction, after the end of the reaction, slowly dropping 0.1N hydrochloric acid to pH6.5 - 7.0, reduced pressure concentration after the clip 90 - 95% of the solvent, then adding 500 ml tap water, stirring crystallization 2 - 3 hours, filtering, washing, drying, so as to further the original crude 92.2g, HPLC containing 98.0%, the weight yield of 92.2%; and then added to the above crude product in 600 ml alcohol, heating to dissolve, adding 5g activated carbon, reflux decoloring 1 - 1.5 hour, take advantage of the heat filtering, the filter cake is about 80 ml alcohol-soaking, the combined filtrate and wash liquid, concentrating at normal pressure to recover 85% alcohol, and then the system cooling to 0 - 5 °C, stirring crystallization 2 - 3 hours, filtering, cake 10 ml 50% ethanol solution of washing, 70 °C following drying, so as to further the original 84.0g, HPLC content 99.4%, the weight yield of 84.0%.
References:
CN106496297,2017,A Location in patent:Paragraph 0013; 0017; 0021
63-05-8
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$32.00/1mg
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975-57-5
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26614-48-2
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