関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 5-Methoxyanthranilic acid | HCID 277930 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-methoxy-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 294479 | 96.1% |
反応手順
To a solution of 2-amino-5-methoxy-benzoic acid (1.2 g, 7 mmol) in anhydrous THF (50 mL) triethylamine (1.0 mL, 7 mmol) was added and the mixture was cooled down to 0° C. Then triphosgene (2.0 g, 7 mmol) was added portion wise and the reaction allowed to reach room temperature and left stirring for 18 hours. 1 mL of H2O was carefully added to the mixture and the solvent was removed under reduced pressure. The residue was precipitated from H2O, affording 1.3 g of the titled compound (96% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08865704B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-7c7a062bdac74258ab0cac3740fa6835 |
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| 出典メモ | uspto-grants-2014_10 |
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