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2,2,2-Trifluoroethanol → CH2=C(CF3)CF2Och2CF3
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | Tributylamine | HCID 7622 | — |
| 反応物 | CH2=C(CF3)CF2Oso2F | HCID 87741755 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | CH2=C(CF3)CF2Och2CF3 | HCID 85887659 | 30% |
反応手順
A 100 ml flask is charged with tributylamine (15 g), diglyme (20 ml) in a dry box. 2,2,2-Trifluoroethanol (8.05 g) is added to the mixture. CH2═C(CF3)CF2OSO2F (19.5 g) is added dropwise while the mixture is cooled in an ice-water bath. The resulting mixture is stirred at room temperature for 3 hours. The mixture is then distilled to give a liquid, which is redistilled (spinning band column) giving 5.8 g CH2═C(CF3)CF2OCH2CF3, b.pt. 85-86° C., a yield of 30%. Less pure fractions are not included in the yield calculation.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07531689B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-29061fff52f645fda0d950a48120b2ac |
| 出典メモ | uspto-grants-2009_05 |