Iodine → 7-Methylisoquinolin-1(2H)-one
反応式
II.[N:3]([CH:6]=[CH:7][C:8]1[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=1)=[C:4]=[O:5]>ClC1C=CC=CC=1Cl>[CH3:14][C:11]1[CH:10]=[C:9]2[C:8]([CH:7]=[CH:6][NH:3][C:4]2=[O:5])=[CH:13][CH:12]=1参加物
4
反応条件
- 温度
- 180 °C
実験手順
Iodine (0.63 g, 2.51 mmol) is added to a solution of 1-(2-isocyanato-vinyl)-4-methyl-benzene (ca. 20 g, 125.6 mmol) in o-dichlorobenzene (125 mL), then is heated to reflux (180° C.) overnight. The mixture is cooled to room temperature then concentrated to dryness. The residue is purified by column chromatography eluting with 40% EtOAc/hexanes. The product (6.23 g, 39.1 mmol) is obtained as a tan solid.
後処理
- temperatureis heated
- temperatureThe mixture is cooled to room temperature
- concentrationthen concentrated to dryness
- customThe residue is purified by column chromatography
- washeluting with 40% EtOAc/hexanes
出典と根拠
- ORDレコード
- ord-551e278571664f97bbdf9be893b956d7
- 出典データセット
- uspto-grants-2001_08
- 特許番号
- US06281227B1
反応ノート
読み込み中…