関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1,1,3,3,3-Pentafluoropropene | HCID 69647 | — |
| 触媒 | Di-tert-butyl peroxide | HCID 8033 | — |
| 生成物 | 2,2,4,4,4-Pentafluorobutan-1-ol | HCID 10329622 | 77% |
反応手順
Under nitrogen, into a quartz reactor equipped with a dry-ice condenser was added anhydrous methanol (100 g, 3.10 mol) and di-tertiarybutylperoxide (3.95 g, 0.015 mol). The quartz reactor tube was placed in a Rayonet UV photochemical reactor and HFC 1225, CF3CH═CF2 (57.9 g, 0.438 mol) was added drop-wise via a dry-ice condenser (−78° C.) over a period of ˜5 hours while being irradiated at 254 nm. After complete addition, the reaction mixture was irradiated for additional hour. Then the reaction mixture was concentrated under reduced pressure, the residue (˜65 g) was mixed well with 120 mL aq. Na2SO3 (20%), separated the lower layer, and washed with brine (40 mL). The crude product was then distilled under reduced pressure (24-28 mm Hg) to afford 55 g CF3CH2CF2CH2OH (yield 77% based on HFC 1225).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06673976B1 |
|---|
| 出典データセット | uspto-grants-2004_01 |
|---|
| ORD ID | ord-2446fb5909434dbaa40d4f451f844b20 |
|---|
| 出典メモ | uspto-grants-2004_01 |
|---|