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-tri-n-butylstannyl-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 this temperature for 20 minutes. A 10% sodium thiosulfate aqueous solution and ethyl acetate were added to this mixture. The organic layer was separated, washed with saturated saline, 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 | US08513287B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-82d95be981254478b30de3c280c47d74 |
| Source note | uspto-grants-2013_08 |