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Triphosgene → 6-Bromo-1,4-dihydro-2H-3,1-benzoxazin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 2-Amino-5-bromobenzenemethanol | HCID 11030874 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-Bromo-1,4-dihydro-2H-3,1-benzoxazin-2-one | HCID 25918963 | 96% |
反応手順
To a solution of (2-amino-5-bromophenyl)methanol (772 mg, 3.8 mmol) in 15 ml THF was added triphosgene (1.03 g, 3.8 mmol) under nitrogen. After precipitation of a colorless solid, stirring was continued for 20 min before water was added. The solution was extracted several times with ethyl acetate. The combined organic layers were washed with brine, dried over MgSO4 and evaporated, affording 6-bromo-1H-benzo[d][1,3]oxazin-2(4H)-one (830 mg, 3.64 mmol, 96%) as colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541404B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-832a93207d004a2982842647434dcf26 |
| 出典メモ | uspto-grants-2013_09 |