HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 66774323, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 13406056 | HCID 13406056 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 66774323 | HCID 66774323 | — |
Reaction Steps
Compound 4 is O-Acetylated using well known literature procedures (Protective Groups in Organic Synthesis, 3rd edition, 1999, pp. 150-160 and references cited therein and in Greene, T. W. and Wuts, P. G. M., eds, Wiley-Interscience, New York.) Acetic anhydride (2 to 2.5 eq.) and triethylamine (4 eq.) is added to a solution of 4 (1 eq.) and N,N-dimethylaminopyridine (0.1 eq.) in anhydrous pyridine. After stirring at room temperature for 1 hour the mixture is treated with methanol to quench excess acetic anhydride and evaporated. The residue is redissolved in ethyl acetate, washed extensively with aqueous NaHCO3, dried over anhydrous Na2SO4, filtered, and evaporated. The compound is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696345B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-5acd14e5baeb4c4faeb8e76bf681e22a |
| Source note | uspto-grants-2010_04 |