HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 178516139, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 178516505 | HCID 178516505 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178516139 | HCID 178516139 | 57.6% |
Reaction Steps
Iodine (8.16 g, 32.1 mmol) was added in five portions to a solution of 2-(trifluoromethyl)pyridin-4-ol (5 g, 30.65 mmol) and K2CO3 (4.66 g, 33.7 mmol) in methanol (34 mL) at 0° C. and the resulting mixture was stirred at room temperature for 20 h. The solution was washed with saturated aqueous sodium sulfite then acetic acid (10 mL) was added and the solution was extracted with ethyl acetate, dried (Na2SO4), filtered, concentrated under vacuum and the residue was purified on a silica gel column to give 5-iodo-2-(trifluoromethyl)pyridin-4-ol (5.1 g, 57%). Retention time (min)=1.761, method [1], MS (ESI) 290.9 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450363B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-02925264b05c485297a242a62e2a4b48 |
| Source note | uspto-grants-2013_05 |