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Acrylonitrile → 6-(2-cyanoethyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acrylonitrile | HCID 7855 | — |
| 反応物 | CID 37314 | HCID 37314 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-(2-cyanoethyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide | HCID 11300176 | 97% |
反応手順
108 g (0.5 mol) of 6H-dibenz-[c,e][1,2]-oxaphosphorin-6-one are heated to 165° C. with stirring and under an inert-gas atmosphere, and 26.5 g (0.5 mol) of acrylonitrile are added dropwise over 4 hours. The mixture is stirred further at this temperature for 1 hour and then cooled, giving 134 g of a resinous composition. Digestion with a little acetonitrile produces 130 g of 6-(2-cyanoethyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide, which, after recrystallization from a little acetonitrile, has a melting point of 120-123° C. The yield is 97% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05990337 |
| 出典データセット | uspto-grants-1999_11 |
| ORD ID | ord-294e6cde76614941a4495e20ac2e259e |
| 出典メモ | uspto-grants-1999_11 |