化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 53417180、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzoic acid, 3,5-dibromo- | HCID 12063 | — |
| 反応物 | Ethane, azido- | HCID 79118 | — |
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Thionyl Chloride | HCID 24386 | — |
| 生成物 | HCID 53417180 | HCID 53417180 | — |
反応手順
The solution of 3,5-dibromobenzoic acid (26 g, 93 mmol) in SOCl2 (100 mL) was heated at reflux for 2 h, concentrated, diluted with dry DCM (300 mL) and added slowly to a stirred solution of N,O-dimethylhydroxylamine hydrochloride (9.75 g, 100 mmol) and EtN3 (28 g, 277 mmol) in dry DCM (300 mL) at 0° C. The solution was stirred for 1 h at rt, poured into water and the organic layer was separated. The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated to give crude compound P37a (28 g, 93%) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08946446B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-a71840bae54548e9944a5090f50bb903 |
| 出典メモ | uspto-grants-2015_02 |