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2-Amino-6-chlorobenzoic acid → 5-chloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-6-chlorobenzoic acid | HCID 75071 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-chloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 639058 | 250.3% |
反応手順
To a stirred warm (50° C.) solution of 2-amino-6-chlorobenzoic acid (2.00 g, 11.7 mM) in tetrahydrofuran (20 mL) was added bis(trichloromethyl)carbonate (1.20 g, 4.10 mM). A vigorous gas evolution ensued along with the formation of a precipitate. The reaction mixture was allowed to cool to room temperature and the precipitate was collected by filtration and washed with ether. Air drying gave the title compound as a tan solid (2.0 g, 87%); MS(CI): 198 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733910 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-11cb73d43db14970822d1f7987ae94cd |
| 出典メモ | uspto-grants-1998_03 |