関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 2-Amino-6-methoxybenzoic Acid | HCID 2735357 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Methoxy-2H-3,1-benzoxazine-2,4(1H)-dione | HCID 10750295 | 283.3% |
反応手順
To a stirred warm (50° C.) solution of 2-amino-6-methoxybenzoic acid (2.70 g, 16.2 mM) in tetrahydrofuran (25 mL) under a nitrogen atmosphere was added bis(trichloromethyl)carbonate (1.60 g, 5.38 mM), whereupon a tan precipitate formed. The reaction mixture was maintained at 50° C. for 30 min, cooled, rewarmed to 50° C. for 30 min, filtered cool and dried to provide the title compound (2.95 g, 94.6%) as an off-white solid; MS(CI): 194 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05733910 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-566fc546dbbd4317ba914612b55bdb28 |
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| 出典メモ | uspto-grants-1998_03 |
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