Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59444764 | HCID 59444764 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59444760 | HCID 59444760 | 93.2% |
Reaction Steps
Triethylamine (35.6 μl, 246 μmol), acetic anhydride (11.6 μl, 123 μmol) and 4-dimethylaminopyridine (3.0 mg, 24.6 μmol) were added to an anhydrous dichloromethane (2 ml) solution of (4R,7R,8S,9E,11S,12S)-4,7,8-trihydroxy-7,11-dimethyl-12-[(1E)-1-methylbuta-1,3-dien-1-yl]-oxacyclododec-9-en-2-one (40.0 mg, 123 μmol) at 0° C. and the reaction solution was stirred at the same temperature for one hour. The reaction solution was poured into a saturated sodium hydrogen carbonate aqueous solution, and the reaction solution was diluted with ethyl acetate and washed with distilled water and brine sequentially, and after dried over anhydrous sodium sulfate, the drying agent was filtered off and the organic layer was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (Merck, commercial name Silica Gel 60, 230-400 mesh; hexane:diethyl ether=1:2) to obtain the title compound (42 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07884128B2 |
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| Source dataset | uspto-grants-2011_02 |
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| ORD ID | ord-017de5bf2a5b4c6da6c78e8088949434 |
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| Source note | uspto-grants-2011_02 |
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