HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22616346, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 12052213 | HCID 12052213 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 22616346 | HCID 22616346 | 94% |
Reaction Steps
To the mixture of Compound 2a (1.2 g, 3.6 mmol) obtained in Step A of Example 2 and p-toluenesulfonic acid monohydrate (1.2 mg, 0.0063 mmol) were added water (70 mL) and toluene (140 mL ), followed by refluxing for 4 hours. The mixture was allowed to cool, the mixture was extracted with toluene, and the extract was washed with a saturated aqueous solution of sodium bicarbonate and then with brine. The mixture was dried over sodium sulfate, the solvent was evaporated, and the residue was purified by silica gel column chromatography (eluted with hexane/ethyl acetate=2/1) to give Compound 16 (0.88 g, 94%) as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376535B2 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-e676341a128347c5a73d940c927872c2 |
| Source note | uspto-grants-2002_04 |