Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
p-Toluenesulfonic acid → Triphenylphosphine Oxide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester | HCID 70670 | — |
| 반응물 | 2-(1-hydroxy-1-methoxymethyl)-5-(phenylmethoxy)-4(1H)-pyridinone | HCID 14182517 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Triphenylphosphine Oxide | HCID 13097 | — |
| 생성물 | 3-[1,4-Dihydro-4-oxo-5-(phenylmethoxy)-2-pyridinyl]-2-propenoic acid, ethyl ester | HCID 86742168 | — |
반응 단계
0.5 g of p-toluenesulfonic acid, 6.26 g of 2-(1-hydroxy-1-methoxymethyl)-5-(phenylmethoxy)-4(1H)-pyridinone and 8.35 g of carbethoxymethylenetriphenylphosphorane were stirred for 3 hours in 100 ml of dioxane at 70° C. A clear, dark-colored solution was formed. Evaporation of the solvent in vacuo yielded an oily residue of the title compound and triphenylphosphine oxide. The residue was dissolved in 30 ml of isopropanol and crystals of product began to separate. After standing in a refrigerator overnight, the crystals were filtered off, washed with ether and recrystallized from isopropanol. Yield: 5.72 g, melting point 188° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04743685 |
| 출처 데이터셋 | uspto-grants-1988_05 |
| ORD ID | ord-a908bb603e0146ed9a83ce1678d4b7aa |
| 출처 메모 | uspto-grants-1988_05 |