4-Toluenesulfonyl chloride → HCID 57799575、化合物

反応式

[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:11](=[C:12]([O:14][CH3:15])[CH:13]=1)[C:10](=[O:16])[C:9](=[N:17]O)[CH2:8]2.C1(C)C=CC(S(Cl)(=O)=[O:26])=CC=1>O>[C:9]([CH2:8][C:7]1[CH:6]=[C:5]([O:4][CH3:3])[CH:13]=[C:12]([O:14][CH3:15])[C:11]=1[C:10]([OH:16])=[O:26])#[N:17]

参加物

反応条件

温度: 50 °C

実験手順

To a solution of NaOH (3.4 g, 85 mmol) in H2O (50 ml) was added of 5,7-Dimethoxy-indan-1,2-dione 2-oxime (5.0 g, 22.6 mmol). The mixture was heated to 50° C. Then p-Toluenesulfonyl chloride (5.7 g, 30 mmol) was added in portions to the mixture. The mixture was heated at 80° C. for 15 min. After cooling carefully to room temperature, the precipitate (a little) was removed from the mixture. Mother liquid was acidified by concentrated HCl to PH=3-4 and precipitate was formed. The precipitate was collected and dried to give product (3.5 g, 70%). LC-MS: m/e 220 (M−1).