Oxalyl chloride → Benzofuro[3,2-d]pyrimidine-2,4(1H,3H)-dione
反応式
[NH2:1][CH:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH:3]1[C:11]([NH2:13])=[O:12].C(Cl)(=O)[C:15](Cl)=[O:16]>C1(C)C=CC=CC=1>[NH:1]1[C:2]2[C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=3[O:4][C:3]=2[C:11](=[O:12])[NH:13][C:15]1=[O:16]参加物
4
反応条件
- 温度
- 115 °C
実験手順
To a stirred solution of 3-amino-2,3-dihydrobenzofuran-2-carboxamide (82.2 mg, 0.461 mmol, 1.0 eq.) in anhydrous toluene (8 mL) under an inert atmosphere was added oxalyl chloride (70.2 mg, 553 μmol, 1.2 eq.) in a dropwise manner. The resulting mixture was heated to reflux (115° C.) for 4 hours whereupon it was cooled and stirred for a further 16 hours. The crude reaction mixture was concentrated to half of its volume and filtered to give a colorless solid (41.5 mg, 45%).
後処理
- temperatureThe resulting mixture was heated
- temperaturewas cooled
- customThe crude reaction mixture
- concentrationwas concentrated to half of its volume
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-d5c02217c7884951bb6adf80a3ddd063
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08921361B2
反応ノート
読み込み中…