7-DEHYDROCHOLESTERYL BENZOATE synthesis
- Product Name:7-DEHYDROCHOLESTERYL BENZOATE
- CAS Number:1182-06-5
- Molecular formula:C34H48O2
- Molecular Weight:488.74
Yield:1182-06-5 120 g
Reaction Conditions:
with dmap;triethylamine in dichloromethane at 25; for 4 h;Inert atmosphere;
Steps:
1.1 1) Preparation of 3-benzoate-7-dehydrocholesterol (compound A):
add 100 g of 7-dehydrocholesterol to a 2L three-necked flask, add 1L of dichloromethane, stir and dissolve, and then add 1.1 times 7 -Dehydrocholesterol molar amount of benzoyl chloride (40.2g), after stirring evenly, add dropwise 1.2 times 7-dehydrocholesterol molar amount of triethylamine (31.2g); after the dropwise addition, add 3.2g of DMAP, Under nitrogen protection, the reaction was carried out with stirring at room temperature (25 °C ± 2 °C). After the reaction for 4 h, samples were taken for TLC monitoring. Dry with 100 g of anhydrous sodium sulfate, concentrate under reduced pressure at room temperature to 1/3 the volume of the original mixed solution, then add 300 ml of methanol to the concentrated solution to replace dichloromethane, a solid is precipitated, freeze at -15 °C for 4 hours, suction filtration, Dry to obtain solid 120g, and the solid obtained is 3-benzoate-7-dehydrocholesterol;
References:
CN114213301,2022,A Location in patent:Paragraph 0038-0040
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