HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 90408799, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 90408487 | HCID 90408487 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 90408799 | HCID 90408799 | 92.1% |
Reaction Steps
Thionyl chloride (67 mL, 922 mmol) is added dropwise to a solution of 6-(1-hydroxy-2-methylpropan-2-ylamino)-5-methyl-2-(4-bromobenzyl)-2H-pyrazolo[3,4-d]pyrimidin-4(5H)-one (134 g, 330 mmol) in DMF (800 mL). The reaction mixture is stirred at room temperature until the reaction is complete. The mixture is poured into cold water, and then adjusted to pH 8-9 with ammonium hydroxide aqueous solution. After filtration, the obtained solids are washed with water, and then dried under vacuum to give 118 g of product (yield: 92%). MS (ESI) 388.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073936B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-baf618cc872e40109b21a10b32554f6b |
| Source note | uspto-grants-2015_07 |