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Triethylamine → Methyl 5-(2,2-difluoroethoxy)-2-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,2-Difluoroethan-1-ol | HCID 136187 | — |
| 反応物 | 2,8,9-Triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo(3.3.3)undecane | HCID 4571243 | — |
| 反応物 | 5-Fluoro-2-nitrobenzoic acid methyl ester | HCID 5152049 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 5-(2,2-difluoroethoxy)-2-nitrobenzoate | HCID 59587324 | 92.5% |
反応手順
8.53 g of 2,2-difluoroethanol are added to a solution of 17.31 g of methyl 5-fluoro-2-nitrobenzoate, 9.64 g of NEt3 and 32.71 g of 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane in 250 ml of anhydrous THF. The mixture is stirred at AT for 30 min. The solvent is evaporated under reduced pressure. Water is added and extraction is carried out with AcOEt. The extract is washed with a 1N aqueous HCl solution, with water and then with a saturated NaCl solution. It is dried over MgSO4 and filtered, and the solvent is evaporated under reduced pressure to give 21 g of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846654B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-6a6caacef79c480cb678629b6f435790 |
| 出典メモ | uspto-grants-2014_09 |