関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,6-Triiodophenol | HCID 11862 | — |
| 反応物 | Diethyl bromomalonate | HCID 69637 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Diethyl 2-(2,4,6-Triiodophenoxy)-1,3-propanedioate | HCID 15343336 | 64% |
反応手順
A stirred mixture of 70.8 g (0.15 mol) of 2,4,6-triiodophenol, 39.0 g (0.15 mol) of diethyl bromomalonate and 20.7 g (0.15 mol) of milled anhydrous potassium carbonate in 200 ml of dry dimethylformamide was heated at 100° C. under argon for 5 hours. The mixture was cooled and concentrated in vacuo. The resulting residue was combined with 300 ml of ice-cold water and the oily product was extracted with ethyl acetate (1×300 ml), 3×100 ml). The combined ethyl acetate extracts were dried (MgSO4) and concentrated in vacuo to a dark oil. The oil was purified by chromatography (eluted by hexanes to 20% diethyl ether in hexanes) to yield 60.2 g (64%) of product as a light cream-colored solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05620677 |
|---|
| 出典データセット | uspto-grants-1997_04 |
|---|
| ORD ID | ord-171e02d978714c69be10db6b1427fc3a |
|---|
| 出典メモ | uspto-grants-1997_04 |
|---|