HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 25114169, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | HCID 25114168 | HCID 25114168 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 25114169 | HCID 25114169 | 66.6% |
Reaction Steps
To a tetrahydrofuran solution (15 mL) of 2-(4-(5-tributylstannyl-isoxazol-3-ylmethyl)-benzyloxy)-pyridine (5.1 g) described in Manufacturing Example 1-8-1 was added iodine (2.5 g) at 0° C. This mixture was stirred at that temperature for 20 minutes. To the mixture were then added 10% sodium thiosulfate aqueous solution and ethyl acetate. The organic layer was isolated, washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was concentrated, and the residue was purified by silica gel column chromatography (heptane:ethyl acetate=10:1 to 4:1) to obtain the title compound (2.4 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188119B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-471b8dbfde0b4858b7a615ac7c4a8ab4 |
| Source note | uspto-grants-2012_05 |