化工社化工社 化学情報印刷レポート · 研究参考用
Oxalyl chloride → HCID 63379722、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 3-Fluorophenylacetic acid | HCID 67617 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Ethyl 2-amino-2-(hydroxyimino)acetate | HCID 6785548 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 63379722 | HCID 63379722 | 30% |
反応手順
This compound was prepared according to general method 2 with (step I) 2-(3-fluorophenyl)acetic acid (1.03 g; 7.57 mmol) and oxalyl chloride (0.704 mL; 8.33 mmol) in dichloromethane (5 mL) and a few drops of DMF and (step II) ethyl 2-amino-2-(hydroxyimino)acetate (1.0 g; 7.57 mmol) and N,N diisopropylethylamine (2.11 mL; 12.11 mmol) in dichloromethane (10 mL) and (step III) pyridine (18 mL). The crude material was purified by flash chromatography on silica (eluent 20 to 100% ethyl acetate in heptane) to yield 0.555 g (30%) of the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434722B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-48f48f8a6acc4a0991449a455fab8b72 |
| 出典メモ | uspto-grants-2016_09 |