(-)-3-OXO-6-BETA-TRITYLOXYMETHYL-7-ALPHA-BENZOYL-OXY-2-OXABICYCLO[3.3.0!OCTANE synthesis
- Product Name:(-)-3-OXO-6-BETA-TRITYLOXYMETHYL-7-ALPHA-BENZOYL-OXY-2-OXABICYCLO[3.3.0!OCTANE
- CAS Number:101208-17-7
- Molecular formula:C34H30O5
- Molecular Weight:518.6
![2H-Cyclopenta[b]furan-2-one, hexahydro-5-hydroxy-4-[(triphenylmethoxy)methyl]-, (3aR,4S,5R,6aS)-](/CAS/20210305/GIF/62939-85-9.gif)
Yield:-
Reaction Conditions:
at 30; for 4.5 h;Temperature;
Steps:
14 One-pot Preparation of (-) Corey lactone benzoate
Add 30L of pyridine to the reactor with the filter element at the bottom, add (a) 4kg (leq) of the Corey lactone diol while stirring, add 7.13kg (1. leq) of triphenylchloromethane, and control the temperature at 20°C for 12h to complete In the reaction, 2.82 L (1.05 eq) of benzoyl chloride was added dropwise and the reaction was allowed to proceed at a controlled temperature of 30° C. for 4.5 h to complete the reaction; 44 L of pure water was added to the reaction vessel and stirred for 2 h to obtain a suspension. Nitrogen gas was introduced into the reaction vessel and passed through the reactor. The bottom of the filter will be suspended hydraulic filter, and then add isopropanol 40L to the reaction vessel, heated to reflux for 1h, the liquid pressure filter to obtain a solid powder; add 60L acetonitrile to the reaction vessel, add 30L of 3mol/L hydrochloric acid aqueous solution dropwise, control Temperature 45 ° C reaction 3.5h to complete reaction, the reaction system was cooled to 10 ° C, was added saturated aqueous sodium carbonate and neutralization reaction to ΡΗ = 7; the solvent acetonitrile in the reaction vessel was distilled off, and the resulting crude product was obtained by pressure filtration; 40K n-propyl ether was added to the reaction vessel, and the mixture was heated to reflux for 3 h, and then pressed and dried to give the product (-) Corey lactone benzoate, 6.4 Kg, a yield of 93.59%, and a purity of 99.03%.
References:
CN107935975,2018,A Location in patent:Paragraph 0111; 0115; 0125; 0129; 0134; 0135; 0141
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![((3aR,4S,6aS)-5-acetoxy-2-oxohexahydro-2H-cyclopenta[b]furan-4-yl)Methyl acetate](/CAS/20150408/GIF/62939-82-6.gif)
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