Diphosgene → 1H,2H,4H-thieno(2,3-d)(1,3)oxazine-2,4-dione
反応式
[NH2:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([O:9][CH3:10])=[O:8].[OH-].[K+].ClC(OC(Cl)(Cl)Cl)=[O:15]>O>[NH:1]1[C:2]2[S:3][CH:4]=[CH:5][C:6]=2[C:7](=[O:8])[O:9][C:10]1=[O:15]参加物
5
反応条件
- 温度
- 90 °C
実験手順
Methyl 2-amino-thiophene-3-carboxylate (5 g, 31.72 mmol) was added to a solution of potassium hydroxide (3.55 g, 63.45 mmol) in 10 mL water. The solution was heated at 90° C. until to get a clear solution. The solution was then cooled to 0° C. and trichloromethyl chloroformate (5.74 mL, 47.57 mmol) was added slowly. The solution was allowed to come to room temperature and further stirred for 30 min. The precipitated solid was collected by vacuum filtration to yield 4.7 g (88%) of 1H-thieno[2,3-d][1,3]oxazine-2,4-dione. MP 233° C. 1H-NMR (DMSO-d6) δ 7.15 (d, J=6.0 Hz, 1H), 7.19 (d, J=6.0 Hz, 1H) ppm.
後処理
- customto get a clear solution
- temperatureThe solution was then cooled to 0° C.
- customto come to room temperature
- filtrationThe precipitated solid was collected by vacuum filtration
出典と根拠
- ORDレコード
- ord-2b08671b5da9486f9b882307b563774d
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07365200B2
反応ノート
読み込み中…