化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Methyl 4-(2-methoxy-2-oxoethyl)-3-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methyl chloroacetate | HCID 7295 | — |
| 反応物 | Methyl 3-nitrobenzoate | HCID 69260 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 4-(2-methoxy-2-oxoethyl)-3-nitrobenzoate | HCID 22567524 | — |
反応手順
54.3 g of methyl 3-nitro-benzoate and 29.0 g of methyl chioroacetate are dissolved in 100 ml of dimethylformamide and this solution is added dropwise at −10° C. to a solution of 78.5 g of potassium tert.butoxide in 500 ml of dimethylformamide. The mixture is stirred for another 10 minutes at ambient temperature and after this time the solution is poured onto 350 ml of concentrated hydrochloric acid in 2 l of iced water. The solution is stirred for 0.5 hours and the precipitate obtained is suction filtered and washed with water. The product is recrystallised from 150 ml of methanol and dried in vacuo at 40° C. Yield: 48.3 g (51% of theoretical), contains about 20% of methyl 6-methoxycarbonylmethyl-3-nitro-benzoate
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858641B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-1ccfac4f8afb4c33b7e6c03d11b4ea37 |
| 出典メモ | uspto-grants-2005_02 |