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ChemicalBook CAS DataBase List Chlormadinone acetate
302-22-7

Chlormadinone acetate synthesis

7synthesis methods
-

Yield:302-22-7 97.8%

Reaction Conditions:

with toluene-4-sulfonic acid;acetic acid in chloroform at 40 - 45;Solvent;

Steps:

D D. Preparation of chlorprogesterone acetate
In a 2000 ml three-necked bottle, 100 g of the above-mentioned homemade chloride and 1000 ml of glacial acetic acid were added, 50 g of acetic anhydride, 2 g of p-toluenesulfonic acid were added under stirring, and then slowly heated to 40-45° C., and the reaction was incubated for 8 to 12 hours while stirring. Confirm the end of the reaction. After the reaction, add 10 ml of 30% liquid base to neutralize the strong acid, then concentrate under reduced pressure to recover 90-85% glacial acetic acid. Finally add 600 ml of tap water, cool down to 10-15°C, stir and crystallize 2-3 hours, filtration, washing to neutrality, filter cake drying below 70 ° C, to obtain crude acetate acetate progesterone 114.2g, HPLC content of 98.8%; filtrate and lotion merger, recovery of residual solvent into the waste water treatment tank; The crude product was recrystallized by decolorization of alcohol and activated charcoal according to a conventional method to obtain 97.8 g of chloramphenicol acetate, having a melting point of 208-212° C., HPLC containing 99.5%, and a yield of 97.8%.

References:

Hunan Kerui Bio-pharmaceutical Co., Ltd.;Gan Hongxing;Zuo Qianjin;Hu Aiguo;Xie Laibin CN107698645, 2018, A Location in patent:Paragraph 0016; 0019; 0022

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