HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178437889, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 178437888 | HCID 178437888 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178437889 | HCID 178437889 | — |
Reaction Steps
To a mixture of 1-cyclopentyl-3-ethyl-6-(hydroxymethyl)pyrazolo[3,4-d]pyrimidin-4-one (1.0 g, 3.8 mmol), CH2Cl2 (25 mL) and triethylamine (0.77 g, 7.6 mmol) at -50° C. was added methanesulfonyl chloride (0.44 g, 3.8 mmol) in CH2Cl2 (5 mL). The reaction mixture was stirred for 1 hour, CH2Cl2 and water were added and the organic layer was separated, dried over MgSO4, filtered and concentrated in vacuo to afford 1.28 g of crude product. The crude product was combined with that from a similar experimental run and the mixture was recrystallized from ether (2×) to afford 1-cyclopentyl-3-ethyl-6-(methylsulfonyloxymethyl)pyrazolo[3,4-d]pyrimidin-4-one, m.p. 138°-140° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05656629 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-8bba124735d241489aae1b06b2d52724 |
| Source note | uspto-grants-1997_08 |