HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 12110021, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 22734123 | HCID 22734123 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 12110021 | HCID 12110021 | 62.2% |
Reaction Steps
p-Toluenesulfonic acid (0.8 g) was added to a suspension of Compound 45a (1.0 g) obtained in Step A of Example 45 in toluene (27 ml), followed by heating under reflux for 30 minutes. After being allowed to stand for cooling, a saturated aqueous solution of sodium bicarbonate was added to the reaction solution for neutralization, followed by extraction with ether. The organic layer was washed with a saturated saline and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The resultant residue was purified by silica gel column chromatography (chloroform/methanol=20/1) to give Compound 67 (0.59 g, 62.2%) as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06716987B1 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-1bcaba57e6274753ae8dab949827dd33 |
| Source note | uspto-grants-2004_04 |