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Hydrochloric Acid → 4-(2-Methyl-cyclopentylamino)-3-nitro-benzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Methylcyclopentylamine | HCID 409747 | — |
| 反応物 | Methyl 4-fluoro-3-nitrobenzoate | HCID 5219721 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(2-Methyl-cyclopentylamino)-3-nitro-benzoic acid methyl ester | HCID 86714452 | 100% |
反応手順
To a solution of 9.32 g of 4-fluoro-3-nitro-benzoic acid methyl ester in 30 ml of abs. DMF was added 16.47 g of potassium carbonate, followed by 5.00 g of 2-methyl-cyclopentylamine. After 16 h at rt, the mixture was poured into water, the pH was adjusted to 5 by the addition of 2 M aqueous hydrochloric acid, and the reaction mixture was extracted with ethyl acetate three times. The combined organic phases were washed with water, dried over sodium sulphate and concentrated to yield 12.74 g (100%) of 4-(2-Methyl-cyclopentylamino)-3-nitro-benzoic acid methyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09156796B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-292a07b7f9884d108e1b60682212dc25 |
| 出典メモ | uspto-grants-2015_10 |