11-a-Hydroxy canrenone methyl ester synthesis
- Product Name:11-a-Hydroxy canrenone methyl ester
- CAS Number:192704-56-6
- Molecular formula:C24H32O6
- Molecular Weight:416.51
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Yield:192704-56-6 80%
Reaction Conditions:
with potassium carbonate in acetone at 0 - 20;
Steps:
2.2
2) Cool the crude acetone solution of the compound represented by the above formula 3 to 0°C,After adding iodomethane(1.5ml, 0.024mol) and potassium carbonate (K2CO3) (5g, 0.036mol) and fully stirred, warmed to room temperature and reacted overnight,TLC detects that the raw materials have completely disappeared. Filter to remove K2CO3,Wash the filter cake with dichloromethane (100ml×3) and combine the organic layers,Spin dry. Dissolve with 250ml of dichloromethane,Then use dilute hydrochloric acid (10% w/w), saturated NaHCO3 solution,Wash with saturated sodium thiosulfate solution and saturated brine,Then dry with anhydrous sodium sulfate, filter,Spin-dry to obtain the crude compound of formula 4 and use it directly in the next step.The crude product of the compound represented by Formula 4 was recrystallized with methylene chloride/toluene to obtain colorless transparent crystals (4 g, yield: 80%).
References:
CN103087139,2016,B Location in patent:Paragraph 0078-0079; 0081-0086
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192704-56-6
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