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Hydrochloric Acid → HCID 178511859、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 反応物 | 2,6-Dichloroisonicotinonitrile | HCID 735906 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178511859 | HCID 178511859 | 57.4% |
反応手順
2,6-dichloropyridine-4-carbonitrile (5 g, 28.9 mmol), methanol (50 ml) and sodium methoxide (0.66 ml, 2.89 mmol) were mixed and stirred at r.t. for 3 h. HCl in EtOH (24% w/w, 10 ml) and cyclopropylamine (3 mL, 43.4 mmol) were added at 0° C., followed by stirring at r.t. o.n. The reaction mixture was concentrated in-vacuo. The isolated residue was treated with cold aq. NaOH (1N, 75 ml) and extracted with EA. The combined organic phase was washed sequentially with aq. NaOH and brine, dried (Na2SO4), filtered and concentrated in-vacuo. The isolated residue was triturated with Et2O to isolate the title compound (3.82 g). 1H-NMR: 7.59 (br. s, 2H), 4.96 (br. s, 2H), 2.60 (m, 1H), 0.90 (m, 2H), 0.69 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07585881B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-e2e554707a4e41a989ac5db57b31e505 |
| 出典メモ | uspto-grants-2009_09 |