化工社化工社 化学情報印刷レポート · 研究参考用
Dibromodifluoromethane → Benzyl 6,6-difluoro-5-methyl-5-hexenoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dibromodifluoromethane | HCID 6382 | — |
| 反応物 | Hexamethylphosphorous triamide | HCID 15355 | — |
| 反応物 | Benzyl 5-oxohexanoate | HCID 12473771 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | Benzyl 6,6-difluoro-5-methyl-5-hexenoate | HCID 19793833 | — |
反応手順
27.85 g Tris(dimethylamino)phosphine was added dropwise to a solution of 17.90 g dibromodifluoromethane in 130 ml diglyme, maintained under a nitrogen atmosphere and ice bath cooling. After stirring for one hour on the ice bath, 8.82 g benzyl 5-oxohexanoate in 70 ml diglyme was added slowly, dropwise. The ice bath was then removed and the reaction mixture stirred for 3 hours at room temperature, allowed to stand overnight, poured into 200 ml ice water and extracted with ether. The ether phase was washed twice with water, dried over sodium sulphate, filtered and concentrated in a rotary evaporator. The residue was distilled under reduced pressure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05248810 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-7f55e0a2549a42539e09fd9289ec2f3a |
| 出典メモ | uspto-grants-1993_09 |