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4-Butoxybenzoic acid → N-(7-chloro-1,8-naphthyridin-2-yl)-4-butoxybenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Butoxybenzoic acid | HCID 72971 | — |
| 反応物 | 7-Chloro-1,8-naphthyridin-2-amine | HCID 85199 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(7-chloro-1,8-naphthyridin-2-yl)-4-butoxybenzamide | HCID 13579409 | 35.2% |
反応手順
The procedure is similar to that described in Example 1, but starting with 4-butoxybenzoic acid (15.5 g), N,N'-carbonyldiimidazole (12.9 g) and 2-amino-7-chloro-1,8-naphthyridine (8.9 g). The product produced by precipitation in water (approximately 18 g; m.p. 140° C.) is purified by chromatography on a column 40 mm in diameter charged with silica (200 g; 0.063-0.2 mm), using methylene chloride as eluant and collecting 60-cc fractions. After concentration to dryness of fractions 8 to 12 at 40° C. under reduced pressure (4 kPa), N-(7-chloro-1,8-naphthyridin-2-yl)-4-butoxybenzamide (6.2 g) is produced, m.p. 197° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04642308 |
| 出典データセット | uspto-grants-1987_02 |
| ORD ID | ord-2336dddbad3b4ae1a27ccf18b239c58f |
| 出典メモ | uspto-grants-1987_02 |