HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 57556922, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Ethyl orthoformate | HCID 31214 | — |
| Reactant | HCID 57556921 | HCID 57556921 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57556922 | HCID 57556922 | 77% |
Reaction Steps
A solution of compound 6 (8.5 g), triethylorthoformate (7.55 mL), p-toluene sulphonic acid (2 g) in THF (75 mL) was stirred at reflux for 4 hours. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in CH2Cl2 (600 mL), washed with 20% NaHCO3 solution and brine, successively, and dried over anhydrous Na2SO4. The solvent was removed under reduced pressure and the crude product was purified by column chromatography on silica gel using a 4:6 mixture of ethyl acetate and pet-ether as the eluent to afford compound 7 (7.9 g, 77%) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776900B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-f6259f380f854fd4bee8ddc7e4d28e6d |
| Source note | uspto-grants-2010_08 |