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Triethylamine → 1,2-Bis-(ethoxycarbonyl)ethyl 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diethyl malate | HCID 24197 | — |
| 反応物 | 5-(2-Chloro-4-(trifluoromethyl)phenoxy)-2-nitrobenzoyl chloride | HCID 3017765 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,2-Bis-(ethoxycarbonyl)ethyl 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoate | HCID 13657069 | 66.7% |
反応手順
To a stirred solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoyl chloride (3.8 g, 0.01 mole) in acetone (10 ml) was successively added diethyl DL malate (1.9 g, 0.01 mole) in acetone (10 ml) and triethylamine (1.01 g, 0.01 mole) in acetone (5 ml). A white precipitate quickly formed. The reaction was heated to reflux for 24 hours. Upon cooling, the reaction was poured in water (75 ml) and extracted twice with methylene chloride (25 ml @). The combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions. The dried solution was stripped of solvent to give 3.56 g of an amber oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04667052 |
| 出典データセット | uspto-grants-1987_05 |
| ORD ID | ord-c3b3c7d9e0284cfe931dcb2aa93c815f |
| 出典メモ | uspto-grants-1987_05 |