HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 11996395, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 11995686 | HCID 11995686 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 11996395 | HCID 11996395 | 6% |
Reaction Steps
Title compound 6A, 1-[3-(3H-Imidazol-4-yl)-phenyl]-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (30 mg, 1.0 eq, 0.11 mmol) was dissolved in DMF (2 ml) and to this was added sodium hydride as a 60% dispersion in oil (5 mg, 1.1 eq, 0.12 mmol), the mixture was then stirred under an inert atmosphere for 20 minutes. To this was added acetyl chloride (7.7 μl, 1.1 eq, 0.12 mmol) the reaction was the stirred for 18 hours and allowed to warm to room temperature. Solvent was then remove in vacuo. The resultant residue was purified using mass-directed preparative HPLC to yield the compound as an off white solid (2.1 mg, 0.0007 mmol, 6%). LCMS: [M+H]+=320, Rt=1.32 min, 87% purity.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071607B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-0cd1125001174f2d916507f97b27a970 |
| Source note | uspto-grants-2011_12 |