HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58677852, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 58677847 | HCID 58677847 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58677852 | HCID 58677852 | — |
Reaction Steps
100 mg (0.21 mmol, purity 80%) of (3S)-1-{2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-5-pyrimidinyl}-3-pyrrolidinol (example XIX, step 3) are dissolved in 2 ml of DMF under argon and, while cooling in an ice bath 8 mg (0.33 mmol) of sodium hydride are added. 32 mg (0.23 mmol) of iodomethane are added dropwise to the suspension, likewise while cooling in an ice bath, and the mixture is stirred at this temperature for 2 hours. 0.5 ml of distilled water is added, and the reaction mixture is chromatographed directly on a preparative HPLC. 35 mg (42% of theory) of the product are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07091198B1 |
| Source dataset | uspto-grants-2006_08 |
| ORD ID | ord-9f4ad61493c44fe6b1cd7d0ba4f2847c |
| Source note | uspto-grants-2006_08 |