ChemicalBook CAS DataBase List Estradiene dione-3-keta

Estradiene dione-3-keta synthesis

6synthesis methods

Product Name:Estradiene dione-3-keta
CAS Number:5571-36-8
Molecular formula:C20H26O3
Molecular Weight:314.43

1,3-Dioxolane, 2,2'-[1,2-ethanediylbis(oxy)]bis-

4544-19-8
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5173-46-6 Synthesis

5173-46-6
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$69.00/5g

107-21-1 Synthesis

107-21-1
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$10.00/25g

5571-36-8
305 suppliers
$5.00/250mg

Yield:5571-36-8 100 kg

Reaction Conditions:

with hydrogenchloride in tetrahydrofuran at -10 - -5;Inert atmosphere;Large scale;Solvent;Reagent/catalyst;

Steps:

1.2-1.3; 2.2-2.3; 3.2-3.3; 4.2; 5.2; 6.2; 6.3; 7.2 (2) Ketal reaction

1300kg of tetrahydrofuran was pumped into the reactor, 100kg of compound of formula (I) was added, under nitrogen protection, it was cooled to -10°C - -5°C, and 80kg of ethylene glycol, 60kg of compound of formula (II), tetrahydrofuran/hydrogen chloride solution (10kg) were added dropwise, the mass concentration of hydrogen chloride is 30% to 35%); after the dropwise addition, the reaction is kept at -10°C to -5°C for 1h to 3h. TLC monitoring, after the reaction is complete, add 6kg of triethylamine to quench the reaction, take the organic phase -0.06Mpa-0.09Mpa and concentrate under reduced pressure to a thick state, cool down to 0°C-5°C for crystallization, filter, take the solid, The wet material of crude 3-ketal product is obtained, which can be directly refined without drying. (3) Refining 800kg of ethyl acetate was pumped into the reaction kettle, put into the wet material of the 3-ketal crude product obtained in step (2), heated to 60-65°C to dissolve, add 5kg of activated carbon to decolorize for 1h, filter out the activated carbon while hot, and the filtrate was transferred to the concentrated crystallization kettle, concentrate under reduced pressure to 300kg in viscous state at 45°C-55°C, cool to 35°C-38°C, slowly add 15%-20% methanol aqueous solution 300kg, ethyl acetate, methanol and water. The mass ratio is 1:0.3:1.2; the ratio of the compound of formula (I) to the total mass of ethyl acetate, methanol and water is 1:5. After the dropwise addition, the temperature was lowered to 0°C to 5°C for crystallization, filtered, and dried at 50°C to 60°C to obtain 100 kg of refined 3-ketal products. Calculated based on the compound of formula (I) as the starting material, the yield of the refined 3-ketal product is 100%, the purity is ≥99%, and the maximum mono-heteropoly is less than or equal to 0.5% (biketal);

References:

CN114456223,2022,A Location in patent:Paragraph 0091; 0094-0099; 0102-0107; 0110-0123; ...

5173-46-6 Synthesis

5173-46-6
246 suppliers
$69.00/5g

107-21-1 Synthesis

107-21-1
1316 suppliers
$10.00/25g

5571-36-8
305 suppliers
$5.00/250mg

References

5173-46-6 Synthesis

5173-46-6
246 suppliers
$69.00/5g

107-21-1 Synthesis

107-21-1
1316 suppliers
$10.00/25g