HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → HCID 178502687, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | HCID 86701834 | HCID 86701834 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178502687 | HCID 178502687 | 83% |
Reaction Steps
To a solution of N,9-dimethoxy-N,1-dimethyl-1,4,5,6-tetrahydropyrazolo[4′,3′:6,7]cyclohepta[1,2-d]pyrimidine-3-carboxamide (583 mg, 1.8 mmol) in CH3CN (35 mL), sodium iodide (550 mg, 3.67 mmol) and trimethylsilylchloride (0.525 mL, 4.14 mmol) were added in sequence. Mixture was stirred for 24 h under argon atmosphere at room temperature then a second portion of sodium iodide (275 mg, 1.8 mmol) and trimethylsilylchloride (0.276 mL, 2.1 mmol) were added in sequence. After 24 h the solvent was evaporated, the residue dissolved with a mixture of DCM/MeOH (4/1) and washed with a saturated aqueous solution of Na2S2O3. The organic layer was dried over Na2SO4. The residue was crystallized from MeOH to give 452 mg (83% yield) of a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916577B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-73cbd6e4b42d41548f3bf47b16536875 |
| Source note | uspto-grants-2014_12 |