関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5-methyl-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 10487522 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Benzyl-6-methyl-isatoic anhydride | HCID 86746432 | — |
反応手順
A solution of 6-methyl-isatoic anhydride (4.5 gm) in DMF (30 ml) was added dropwise to a stirred suspension of 60% sodium hydride (1.0 gm) in DMF (20 ml) under nitrogen atmosphere. The reaction was then warmed to 45° C. and stirred until hydrogen evolution ceased. It was then cooled and a solution of benzyl bromide (4.4 gm) in DMF (10 ml) was added slowly. Stirring was continued for one hour at room temperature and the solution was then evaporated under reduced pressure at 45° C. The resulting solid was suspended in methylene chloride, the insoluble inorganic solid was removed by filtration and the filtrate was evaporated to give 1-benzyl-6-methyl-isatoic anhydride as a crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05412104 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-4c452b40dc494b31bb3fc9080edf4bf9 |
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| 出典メモ | uspto-grants-1995_05 |
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