化工社化工社 化学情報印刷レポート · 研究参考用
Dibromodifluoromethane → Benzyl 8,8-difluoro-7-methyl-7-octenoate
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 7-oxooctanoate | HCID 19793826 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | Benzyl 8,8-difluoro-7-methyl-7-octenoate | HCID 19793855 | — |
反応手順
123 ml (0.68 mol) Tris(dimethylamino)phosphine in 100 ml diglyme was added slowly dropwise to a solution of 26.3 ml (0.34 mol) dibromodifluoromethane in 800 ml diglyme. After stirring for one hour on an ice bath, 43 g (0.17 mol}benzyl 7-oxooctanoate in 100 ml diglyme was slowly added dropwise. The ice bath was removed and the reaction mixture stirred for 40 minutes at room temperature, poured into 1 liter ice-water and extracted with ether. The ether phase was washed twice with water, dried over sodium sulphate, filtered and concentrated. The residue was purified by column chromatography (silica gel hexane/ether=3:1)
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-6a9f947d18fd4b718325c2f1fee21eab |
| 出典メモ | uspto-grants-1993_09 |