Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-[1,1,1,3,3,3-Hexafluoro-2-(methoxymethyl)oxypropan-2-yl]-2-propylphenyl benzyl ether
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2-(4-Benzyloxy-3-propylphenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol | HCID 59201078 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-[1,1,1,3,3,3-Hexafluoro-2-(methoxymethyl)oxypropan-2-yl]-2-propylphenyl benzyl ether | HCID 59201148 | 90.6% |
반응 단계
Sodium hydride (purity: 50%) (38.9 mg, 0.81 mmol) was added to a mixed solution of 2-(4-benzyloxy-3-propylphenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (264.0 mg, 0.67 mmol) in tetrahydrofuran (5 mL) under ice-cooling. Then, chloromethyl methyl ether (65.0 mg, 0.81 mmol) was added, followed by stirring overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate. Then, the organic layer was washed with saturated saline, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel preparative thin-layer chromatography (hexane:ethyl acetate=10:1) to obtain 264.9 mg of the title compound (yield: 90%) as a pale yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08168666B2 |
| 출처 데이터셋 | uspto-grants-2012_05 |
| ORD ID | ord-54a7cfac64824603b128d5c40408eec1 |
| 출처 메모 | uspto-grants-2012_05 |