(7R,8R,9S,10R,13S,14S,17S)-7-(9-hydroxynonyl)-13-methyl-3-oxo-2,3,6,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-1H-cyclopenta[a]phenanthren-17-yl acetate synthesis
- Product Name:(7R,8R,9S,10R,13S,14S,17S)-7-(9-hydroxynonyl)-13-methyl-3-oxo-2,3,6,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-1H-cyclopenta[a]phenanthren-17-yl acetate
- CAS Number:875573-64-1
- Molecular formula:C29H46O4
- Molecular Weight:458.6731
875573-60-7
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Yield:875573-64-1 336 g
Reaction Conditions:
with hydrogenchloride in water at 25 - 30; for 3 h;
Steps:
1.2 (2) Preparation of compound
Transfer all the compound II prepared above to the reaction flask,Add the prepared hydrochloric acid solution (concentrated hydrochloric acid 20.0g + purified water 60.0g), React at 2530 for 3h. When the reaction is complete, add 10wt% sodium carbonate solution (200.0mL),Adjust the pH value to 6-7, stand still for layering, and wash the organic phase with saturated brine once. The organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain 336.0 g of compound III as a pale yellow oil.Detected by HPLC, the 7α configuration product in compound III,The ratio of the 7β configuration product is α: 60.12 wt%, β: 6.21 wt%.
References:
CN112094308,2020,A Location in patent:Paragraph 0053; 0057-0060
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