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Ammonia → Dimethyl 3-benzyl-2-isoxazolin-5-ylphosphonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Phenyl isocyanate | HCID 7672 | — |
| 反応物 | Dimethyl vinylphosphonate | HCID 78376 | — |
| 反応物 | 1-Nitro-2-phenylethane | HCID 80208 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Dimethyl 3-benzyl-2-isoxazolin-5-ylphosphonate | HCID 20062388 | — |
反応手順
13.5 ml (0.124 mol) of phenyl isocyanate, 9.5 g (0.07 mol) of dimethyl vinylphosphonate and 1 ml of triethylamine are introduced into 120 ml of toluene. A solution of 9.3 g (0.062 mol) of 2-phenylnitroethane and 1 ml of triethylamine dissolved in 150 ml of toluene is added dropwise in 5 hours, the mixture is stirred overnight and then for 30 minutes after addition of 30 ml of concentrated aqueous ammonia, precipitated diphenylurea is removed by filtration and washed with ethyl acetate, and the combined organic phases are extracted by shaking successively with water, 2 N hydrochloric acid and water, and are dried and concentrated. 13.9 g of reddish brown oil remain.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05006515 |
| 出典データセット | uspto-grants-1991_04 |
| ORD ID | ord-64ce610377564b8b98bef1e464548e59 |
| 出典メモ | uspto-grants-1991_04 |