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4-Phthalimidomethylthiopyridine → 4-[(2-Methylcarbamoylbenzoyl)aminomethylthio]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Phthalimidomethylthiopyridine | HCID 19079101 | — |
| 反応物 | Monomethylamine methanol | HCID 57454252 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-[(2-Methylcarbamoylbenzoyl)aminomethylthio]pyridine | HCID 19079091 | 35.1% |
反応手順
To a solution of 6.76 g (25.0 mmol) of 4-phthalimidomethylthiopyridine in 100 ml of chloroform, 5 ml of 40% methylamine-methanol solution was added, and the mixture was stirred at room temperature for 3 hours. Additional 5 ml of 40% methylamine-methanol solution was added, and the mixture was stirred at room temperature for 3 hours. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethanol/ethyl acetate =1:10), and the resulting crude product-was crystallized from methylene chloride-diethylether to give 2.645 g of the desired compound (35.1% yield, yellow crystals), mp. 118°-121° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246948 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-4a5162e35a304121b841b3e3f39d8e9f |
| 出典メモ | uspto-grants-1993_09 |