HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 4-t-Butoxy-2,3,6-trifluoro-5-methoxypyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Reactant | 4-t-Butoxy-2,3,6-trifluoro-5-hydroxypyridine | HCID 10656587 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-t-Butoxy-2,3,6-trifluoro-5-methoxypyridine | HCID 10489910 | 85.7% |
Reaction Steps
To a solution of 237 mg (1.07 mmol) of 4-t-butoxy-2,3,6-trifluoro-5-hydroxypyridine, from step 275a above, in 3 mL of anhydrous THF was added 335 mg (1.277 mmol) of triphenyl phosphine and 0.060 mL (1.48 mmol) of methanol. To this solution was added 0.200 mL (1.270 mmol) of DEAD dropwise at room temperature. The reaction was complete in 10 min, so the solvents were removed under vacuum and the residue was purified by flash chromatography on silica gel, eluting with 1:16 ethyl acetate:hexane to give 215.6 mg of the title product as a colorless liquid after removal of the solvent.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05726182 |
| Source dataset | uspto-grants-1998_03 |
| ORD ID | ord-60ba32da8a3a420db576adcfd7bcef8c |
| Source note | uspto-grants-1998_03 |