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Triethylamine → N1-(3-nitro[1,5]naphthyridin-4-yl)-2-methylpropane-1,2-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Methylpropylenediamine | HCID 13128 | — |
| 反応物 | 4-Chloro-3-nitro-1,5-naphthyridine | HCID 13122787 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N1-(3-nitro[1,5]naphthyridin-4-yl)-2-methylpropane-1,2-diamine | HCID 86626700 | 97.4% |
反応手順
1,2-Diamino-2-methylpropane (8.4 mL, 80.0 mmol) was added to a chilled (0° C.) solution of 4-chloro-3-nitro[1,5]naphthyridine (15.2 g, 72.7 mmol) and triethylamine (20.2 mL, 145 mmol) in dichloromethane (350 mL). The reaction mixture was stirred overnight and then concentrated under reduced pressure. The residue was combined with water (300 mL) and heated at reflux with stirring for 1 hour. The reaction mixture was cooled and filtered. The isolated solid was washed with water and then dried under high vacuum to provide 18.5 g of N1-(3-nitro[1,5]naphthyridin-4-yl)-2-methylpropane-1,2-diamine as a bright yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846710B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-1364b9624aaf45ae9988adb32894f8cf |
| 出典メモ | uspto-grants-2014_09 |