化工社化工社 化学情報印刷レポート · 研究参考用
Toluene → 2-(2-fluorobiphenyl-4-yl)-N-methylpropanohydroxamic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| 反応物 | Flurbiprofen Acid Chloride | HCID 11032707 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2-(2-fluorobiphenyl-4-yl)-N-methylpropanohydroxamic acid | HCID 15670529 | — |
反応手順
2-(2-Fluorobiphenyl-4-yl)propionic acid chloride (prepared in the normal manner from 1.75 g of acid, ca 1 ml of oxalyl chloride, toluene, and 3 drops of N,N-(dimethylformamide) was dissolved in tetrahydrofuran (30 ml) and added over 5-10 minutes to a solution of N-Methylhydroxylamine hydrochloride (ca 2 g) in water (5 ml) containing triethylamine (5 ml) at 0°. Solvent was evaporated, and neutral material was isolated with ethyl acetate. Recrystallization from ether-light petroleum (b.pt. 40°-60°) afforded 2-(2-fluorobiphenyl-4-yl)-N-methylpropanohydroxamic acid (1.25 g), m.pt. 125°-126° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04738986 |
| 出典データセット | uspto-grants-1988_04 |
| ORD ID | ord-20759e6e1e2c4715a243d6d81a477b3d |
| 出典メモ | uspto-grants-1988_04 |