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Trifluoroacetonitrile → HCID 178472209、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetonitrile | HCID 67710 | — |
| 反応物 | Ethyl 3-oxovalerate | HCID 78656 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | HCID 178472209 | HCID 178472209 | — |
反応手順
To a mechanically stirred solution of 287 g (1.99 mol) of ethyl propionylacetate in 500 ml of dry DME was added under nitrogen 8.6 g (0.348 mol) of freshly cut sodium. After all sodium had dissolved, 256 g (2.69 mol) of trifluoroacetonitrile was added over a 35 hour period. The reaction mixture was concentrated. The residue was washed with water and extracted into 500 ml of ether. The ether solution was dried and concentrated. The residue was kugelrohr distilled at 67 Pa. and then was redistilled at 67 Pa through a spinning band column. The first fraction (bp 40°-78° C.) was discarded. The next fraction (bp 79°-82° C.) was 151 g (31.6%) of product, nD25 1.4574.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04655816 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-1252b550ae124bd5b158217c426e7714 |
| 出典メモ | uspto-grants-1987_04 |