化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → 2'-Bromo-4'-nitro-1,2,2,3,3,4,4,5,5,6,6-undecafluorocyclohexanecarboxanilide, tetra-n-propylammonium salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Cyclohexanecarboxamide, N-(2-bromo-4-nitrophenyl)-1,2,2,3,3,4,4,5,5,6,6-undecafluoro- | HCID 163772 | — |
| 触媒 | Tetrapropylammonium bromide | HCID 74745 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2'-Bromo-4'-nitro-1,2,2,3,3,4,4,5,5,6,6-undecafluorocyclohexanecarboxanilide, tetra-n-propylammonium salt | HCID 131716799 | 75.9% |
反応手順
2'-Bromo-4'-nitro-1,2,2,3,3,4,4,5,5,6,6-undecafluorocyclohexanecarboxanilide (2.6 grams; 0.005 mole) was dissolved in 50 ml. of acetone and 1N sodium hydroxide (5.0 ml., 0.005 mole) was added all at once. Tetrapropylammonium bromide (1.35 gram; 0.005 mole) was then added and the reaction mixture was stirred until it became one phase. The reaction mixture was then poured over ice/water, and an oily solid separated. It was extracted with diethyl ether, dried over magnesium sulfate, evaporated, and crystallized at -10° C. from water/ethanol. 0.9 gram (25% yield) of the tetra-n-propylammonium salt was obtained, m.p., 86°-87° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04992471 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-e28ce42df09c478ebdb755a6013bbde6 |
| 出典メモ | uspto-grants-1991_02 |