HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 58201194, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | HCID 58201211 | HCID 58201211 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58201194 | HCID 58201194 | 95% |
Reaction Steps
The above di-tert-butyl {4-chloro-3-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl}imidodicarbonate (22 g) was dissolved in methanol (400 ml). Pyridinium p-toluenesulfonate (10 g) was added and the mixture was stirred at room temperature for 16 hours. The reaction solution was concentrated, and water (100 ml) was added to the resulting residue, followed by extraction with ethyl acetate (500 ml). The organic layer was washed with brine, and then dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure to obtain the title compound (19.5 g, 95%) as an amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08158638B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-c75d0952e92d4a9b9ed8576ebc50a9c6 |
| Source note | uspto-grants-2012_04 |