化工社化工社 化学情報印刷レポート · 研究参考用
Formaldehyde → Ethyl 2,2-difluoro-3-hydroxypropanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Ethyl bromodifluoroacetate | HCID 69585 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 2,2-difluoro-3-hydroxypropanoate | HCID 2758828 | — |
反応手順
A mixture of paraformaldehyde (4.5 g, 50 mmol), ethyl difluorobromoacetate (10.2 g, 50 mmol) and activated zinc dust (3.3 g, 40 mmol) in anhydrous tetrahydrofuran was heated under reflux for 0.5 h. Then the mixture was treated with a saturated aqueous solution of ammonium chloride and extracted with diethyl ether. After usual work-up the desired compound ethyl 2,2-difluoro-3-hydroxypropionate was obtained by flash chromatography on silica gel (ethyl acetate:hexane; 25:75) (4.1 g, 53%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05416076 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-07cd20d9a5744d628778aeaa05aa92ac |
| 出典メモ | uspto-grants-1995_05 |