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Allyl bromide → 3-allyl-2,3-dihydro-2-[(4-methylphenyl)imino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Allyl bromide | HCID 7841 | — |
| 反応物 | Lithium hydride | HCID 62714 | — |
| 反応物 | Bas 09531330 | HCID 973891 | — |
| 生成物 | 3-allyl-2,3-dihydro-2-[(4-methylphenyl)imino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one | HCID 23287665 | 52.2% |
反応手順
The reaction procedure of Example 11 was followed except that 900 mg (3.34 mmol) of 2-(4-methylanilino)-4H-pyrido[3,2-e]-1,3-thiazin-4-one, 27 mg of lithium hydride and 404 mg of allyl bromide were used. The resulting residue was then purified through silica gel column chromatography (eluant: chloroform) to obtain 539 mg of 3-allyl-2,3-dihydro-2-[(4-methylphenyl)imino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one (recrystallized from a mixture of ether and hexane) as a low polarity substance and 248 mg of 2-[N-allyl-N-(4-methylphenyl)amino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one (recrystallized from ether) 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-2dbb931eeffe471db5bfdaa048c3d35f |
| 出典メモ | uspto-grants-2000_10 |