化工社化工社 化学情報印刷レポート · 研究参考用
Hydroxylamine → 2,3-Difluoro-6-(trifluoromethyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxylamine | HCID 787 | — |
| 反応物 | 2,3-Difluoro-6-(trifluoromethyl)benzonitrile | HCID 10104456 | — |
| 反応物 | Methanol--water (1/1) | HCID 22242641 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,3-Difluoro-6-(trifluoromethyl)benzamide | HCID 22010119 | — |
| 生成物 | 2,3-Difluoro-N-hydroxy-6-(trifluoromethyl)benzimidamide | HCID 54418213 | — |
反応手順
Into an SUS reaction vessel was placed a mixed solvent of 1.5 L of methanol-water (volume ratio 1:2, the same tap water as that used in Example 2 was used as water) into which 99.09 g (1.50 mol) of 50% hydroxylamine aqueous solution was dissolved beforehand. Into the mixed solvent was added 103.56 g (500 mmol) of 2,3-difluoro-6-trifluoromethylbenzonitrile (I″). The reaction temperature stood at 60° C. for 7 hours and was returned to room temperature. In HPLC analysis of the reaction solution, it was shown that (I″) disappeared, 2,3-difluoro-6-trifluoromethylbenzamidoxime (II′) was mainly produced (yield 63.2%) and 2,3-difluoro-6-trifluoromethylbenzamide (III′) was noticeably produced as a byproduct (yield 16.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06211232B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-84d0e60dca374dd68ebd4b766ca4f0a7 |
| 出典メモ | uspto-grants-2001_04 |