反应详情

Dimethyl sulfate (1.04 ml, 11.0 mmol) was added dropwise to a mixture of potassium carbonate (3.34 g, 24.2 mmol) and 2-amino-4,6-dimethoxybenzoic acid (2.56 g, 11.0 mmol) in dimethylformamide (70 ml) at 0° C. The reaction was stirred for 1 hour, then poured into water. The resulting precipitate was filtered, washed with water and dried in vacuo. The filtrate was extracted with ethyl acetate, and the combined organic extracts were dried (magnesium sulphate) and concentrated in vacuo. The combined solids were dried in vacuo to yield methyl 2-amino-4,6-dimethoxybenzoate (1.8 g, 77% yield) as a yellow crystalline solid:

1. filtrationThe resulting precipitate was filtered
2. washwashed with water
3. customdried in vacuo
4. extractionThe filtrate was extracted with ethyl acetate
5. dry with materialthe combined organic extracts were dried (magnesium sulphate)
6. concentrationconcentrated in vacuo
7. customThe combined solids were dried in vacuo