HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → HCID 10907333, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 22103556 | HCID 22103556 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10907333 | HCID 10907333 | — |
Reaction Steps
To a solution of the title compound of Step (D) (45 mg, 0.075 mmol) in 3 ml of CH3CN, Me3SiCl (41 mg, 0.38 mmol) was added and followed by NaI (57 mg, 0.38 mmol). The mixture was stirred at room temperature for 1.5 hrs. Additional Me3SiCl (32 mg, 0.3 mmol) and NaI (46 mg, 0.3 mmol) were added in twice after stirred for 30 min and 1 hr. 3 ml H2 O and 30 ml EtOAc were added. The organic layer was washed with sat. Na2S2O3, brine, dried and concentrated. The residue was purified by preparative HPLC on an ODS S10 column using 33% solvent A (10% MeOH, 90% H2O, 0.1% TFA) and 67% solvent B (90% MeOH, 10% H2O, 0.1% TFA) to provide the title compound of this Example (23 mg, 60%) as a white solid, m.p. 117°-123° C. (amorphous).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05846990 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-384a150aa69c4b71a0ab34a69e5664b3 |
| Source note | uspto-grants-1998_12 |