Dimethyl Sulfate → HCID 20738653、化合物

反応式

[OH:1][C:2]1[C:3]([CH3:14])=[C:4]([CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:5](O)=[O:6].[C:15]([O-])([O-])=O.[K+].[K+].COS([O:26][CH3:27])(=O)=O>CC(C)=O>[CH3:15][O:1][C:2]1[C:3]([CH3:14])=[C:4]([CH:8]=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12])[C:5]([O:26][CH3:27])=[O:6]

参加物

反応条件

温度: 60 °C

実験手順

To a solution of the crude 3-hydroxy-2-methyl-4-nitrobenzoic acid in acetone (300 mL) was added K2CO3 (15.8 g, 115 mmol) and Me2SO4 (8.7 g, 69 mmol). The mixture was refluxed at 60° C. for 2 h. After the solvent was evaporated in vacuo, the resulting residue was purified by silica gel-column (eluting with PE/EA=10:1) to afford methyl 3-methoxy-2-methyl-4-nitrobenzoate as a yellowish solid (2.7 g, 33% yield, two steps). m/z (ES+APCI)+: [M+H]+226.1.