関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Diethylphosphite | HCID 3780918 | — |
| 反応物 | 1-(5-Bromopentyl)-7-ethoxymethyl-3-methylxanthine | HCID 19689250 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Diethyl [5-(7-ethoxymethyl-3-methylxanthin-1-yl)pentyl]phosphonate | HCID 22446295 | — |
反応手順
4.8 g (0.035 mol) of diethyl phosphite were cooled to 0° C. in 100 ml of dry dimethylformamide and slowly treated with 0.8 g (0.035 mol) of sodium hydride. The solution was stirred at 20° C. for 0.5 hours to complete the deprotonation and then treated with 10 g (0.0268 mol) of 1-(5-bromopentyl)-7-ethoxymethyl-3-methylxanthine, dissolved in a little dimethyl-formamide. After 4 hours at 20° C., the reaction mixture was quenched with a little saturated ammonium chloride solution, concentrated and chromatographed on silica gel (eluent: dichloromethane/methanol 15:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05728686 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-aad289277c9f4d77a324e372db09a54a |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|