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Lithium hydride → HCID 15485506、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium hydride | HCID 62714 | — |
| 反応物 | 3-Methoxybenzyl chloride | HCID 69994 | — |
| 反応物 | 4H-Pyrido[3,2-e]-1,3-thiazin-4-one, 2-[(4-chlorophenyl)amino]- | HCID 4292070 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 15485506 | HCID 15485506 | 22.2% |
反応手順
The reaction procedure of Example 11 was followed except that 2.681 g (9.25 mmol) of 2-(4-chloroanilino)-4H-pyrido[3,2-e]-1,3-thiazin-4-one, 162 mg of lithium hydride, 1.50 g of 3-methoxybenzyl chloride and 40 ml of DMF were used. The resulting residue was then purified through silica gel column chromatography (eluant: chloroform). As a result, 2.288 of 2-[N-(4-chlorophenylimino)-2,3-dihydro-4H-3-(3-methoxybenzyl)pyrido[3,2-e]-1,3-thiazin-4-one (recrystallized from ethanol) was obtained as a low polarity substance, and 843 mg of 2-[N-(4-chlorophenyl)-N-(3-methoxybenzyl)amino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one (recrystallized from a mixture of ethyl acetate and diisopropyl ether) was obtained as a high polarity substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06133258 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-c5ed689f8c674c58a630c28b85b77de5 |
| 出典メモ | uspto-grants-2000_10 |