反应详情

Potassium carbonate(34.55 g) was dissolved in 100 ml of distilled water, 7.30 g of L-glutamine was dissolved in the solution, and 20 ml of acetonitrile was further added to the solution. The reaction mixture was added dropwise with 10.45 g of methacryloyl chloride over about 10 minutes with vigorous stirring, and further stirred for about 2 hours. The reaction mixture was adjusted to pH 1-2 with concentrated hydrochloric acid, saturated with sodium chloride, and extracted 2 times with 100 ml of ethyl acetate. The obtained aqueous layer was extracted 3 times with 100 ml of ethyl acetate/isopropanol=1/1. The ethyl acetate/isopropanol layers were combined, concentrated, and purified on a silica gel column (30 g of silica gel, eluted with chloroform/methanol=2/1). The corresponding fractions were collected and concentrated (colorless syrup, 7.47 g)

1. additionwas further added to the solution
2. extractionextracted 2 times with 100 ml of ethyl acetate
3. extractionThe obtained aqueous layer was extracted 3 times with 100 ml of ethyl acetate/isopropanol=1/1
4. concentrationconcentrated
5. custompurified on a silica gel column (30 g of silica gel, eluted with chloroform/methanol=2/1)
6. customThe corresponding fractions were collected
7. concentrationconcentrated (colorless syrup, 7.47 g)