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Ethylenediamine → N-(2,5-Dimethyl-pyrazolo[1,5-a]pyrimidin-7-yl)-ethane-1,2-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 7-Chloro-2,5-dimethylpyrazolo(1,5-a)pyrimidine | HCID 18406987 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-(2,5-Dimethyl-pyrazolo[1,5-a]pyrimidin-7-yl)-ethane-1,2-diamine | HCID 18406994 | 94.5% |
反応手順
To a stirred solution of 7-chloro-2,5-dimethyl-pyrazolo[1,5-a]pyrimidine (3.0 g, 16.5 mmol) in ethanol (60 mL) was added ethylene diamine (4 mL, 60 mmol). After refluxing 18 hours the reaction was cooled, poured into saturated aqueous sodium bicarbonate, and then washed with ethyl acetate. The aqueous layer was then extracted with 3:7 isopropyl alcohol/chloroform, the combined extracts were dried (Na2SO4) and then concentrated under reduced pressure to give the title compound as an amorphous brown solid (3.2 g, 94%): +APcI MS (M+1)+ 206; 1H NMR (methanol-d4) δ: 6.05 (s, 1H), 6.00 (s, 1H), 3.45 (m, 2H), 2.91 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06476038B1 |
| 出典データセット | uspto-grants-2002_11 |
| ORD ID | ord-90f310a4376644af9f2c95c18f2ef731 |
| 出典メモ | uspto-grants-2002_11 |