Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 4-t-Butoxy-2,3,6-trifluoro-5-methoxypyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 반응물 | 4-t-Butoxy-2,3,6-trifluoro-5-hydroxypyridine | HCID 10656587 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-t-Butoxy-2,3,6-trifluoro-5-methoxypyridine | HCID 10489910 | 85.7% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05726182 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-60ba32da8a3a420db576adcfd7bcef8c |
| 출처 메모 | uspto-grants-1998_03 |