化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → Diethylphosphonomethyl 4-chloro-2-methoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | Diethyl phosphonomethanol | HCID 76513 | — |
| 反応物 | 4-Chloro-o-anisic acid | HCID 93682 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Diethylphosphonomethyl 4-chloro-2-methoxybenzoate | HCID 57457786 | — |
反応手順
A mixture of 4-chloro-2-methoxybenzoic acid (1 mmol), oxalyl chloride (1 mmol), and DMF (0.05 mmol) in 2 mL of CH2Cl2 was stirred at rt for 6 h and then evaporated. To the residue was added 2 mL of CH2Cl2, triethylamine (2 mmol) and diethyl (hydroxymethyl)phosphonate (0.33 mmol) and this mixture was stirred at rt for 16 h and then diluted with water and CH2Cl2. The organic layer was dried (MgSO4) and evaporated. Purification of the residue by silica gel chromatography provided diethylphosphonomethyl 4-chloro-2-methoxybenzoate as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07371739B2 |
| 出典データセット | uspto-grants-2008_05 |
| ORD ID | ord-7e4e9ff495a54311b5a7cda48e9bc141 |
| 出典メモ | uspto-grants-2008_05 |