化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → N-(N-[Bicyclo[2.2.1]hept-2-en-5-ylmethyl]carbamoyl)-2-phenylethenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Phenylethenesulfonamide | HCID 257501 | — |
| 反応物 | N'-(bicyclo[2.2.1]hept-5-en-2-ylmethyl)-N,N-diphenylurea | HCID 12282081 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | N-(N-[Bicyclo[2.2.1]hept-2-en-5-ylmethyl]carbamoyl)-2-phenylethenesulfonamide | HCID 54231290 | — |
反応手順
To a solution of 1.8 g. of 2-phenylethenesulfonamide and 4.8 g. of 1,1-diphenyl-3-(bicyclo[2.2.1]hept-2-en-5-ylmethyl)urea in 20 ml. of N,N-dimethylformamide, is added, with stirring 0.64 g. of a 56.6% dispersion of sodium hydride in mineral oil. The mixture is stirred at ambient temperature overnight, during which time a heavy precipitate forms. To the reaction mixture is then added 200 ml. of ether. After stirring for 15 minutes, the precipitate is filtered off. It is dissolved in 50 ml. of water, and then the crude product is precipitated by acidification usng concentrated hydrochloric acid. It is filtered off and recrystallized from aqueous acetone. The yield is 1.9 g. (56%) of a solid, m.p. 161°-163.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04062960 |
| 出典データセット | uspto-grants-1977_12 |
| ORD ID | ord-0f04b68366f946ca8929ad0918755bef |
| 出典メモ | uspto-grants-1977_12 |