Metandienone synthesis
- Product Name:Metandienone
- CAS Number:72-63-9
- Molecular formula:C20H28O2
- Molecular Weight:300.44
Yield:72-63-9 94.6%
Reaction Conditions:
Stage #1: methyl bromidewith magnesium in tetrahydrofuran at 40 - 45;
Stage #2: Androsta-1,4-diene-3,17-dione in toluene at 50 - 55;
Steps:
2 Example 2
A, preparation of Grignard reagent In a 1000 ml three-necked flask, add 35 g of magnesium powder, 800 ml of tetrahydrofuran, and stir.Insulation at 40-45 ° C into 120 g of methyl bromide,After the completion of the reaction, continue to stir the reaction for 2 to 3 hours.Until the magnesium powder disappears, the Grignard reagent is used; B, preparation of metandienone In a 1000ml three-necked flask, add 100g IDD, 500ml of toluene, and stir to 50~55 °C.Slowly add the above prepared 800ml Grignard reagent solution, about 1-1.5 hours, and continue to stir the reaction for 2 to 3 hours.The end point of the reaction was detected by TLC. After the reaction, 2N hydrochloric acid was slowly added dropwise to PH2-3.After the completion of the dropwise addition, the hydrolysis reaction was continued at 50 to 55 ° C for 2-3 hours, and the hydrolysis was completed by TLC. After the reaction,A mixture of about 90-95% THF and toluene was concentrated under reduced pressure, and the mixture of the recovered THF and toluene was applied.Then, 600 ml of tap water was added to the above residue, and the system was cooled to 5 to 10 ° C, and the mixture was stirred for 2 to 3 hours.Filtration, filter cake washed with tap water to neutral, dried below 70 °C,Got the crude metandienone93.8g,The HPLC content was 98.5%, and the weight yield was 93.8%. C, purification of dehydromethyl testosteroneIn a 1000 ml three-necked bottle, add 100 g of the crude dehydromethyltestosterone prepared in the above step B,500 ml of isopropanol was stirred at 30-35 ° C to completely dissolve it, then 5 g of activated carbon was added and heated to reflux for 1.5-2 hours.Then, the temperature is lowered to 55-60 degrees, filtered while hot, the filter cake is washed with about 100 ml of isopropyl alcohol, and the filter cake is sent to the manufacturer for recycling.The filtrate and the washing liquid are combined and concentrated under normal pressure to recover about 88-90% of isopropanol, and then the system is cooled to -5 to 0 ° C.Stirring for 3 to 4 hours, filtering, recovering the solvent and the mother liquor, and filtering the cake with a small amount of 50% aqueous solution of isopropanol.Drying below 70 °C, 93.8g of metandienone product,The melting point of 165.5 ~ 167.5 ° C, HPLC content of 99.3%, weight yield of 94.6%.
References:
CN109456378,2019,A Location in patent:Paragraph 0043-0049
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