反应 #76727

反应方程式

hydrochloric acid

L-glutamine

Potassium carbonate

sodium chloride

methacryloyl chloride

→

Glutamine-methacrylamide

溶剂

acetonitrile

water

反应条件

后处理

1. 1
   workup.ADDITIONwas further added to the solution
2. 2
   萃取extracted 2 times with 100 ml of ethyl acetate
3. 3
   萃取The obtained aqueous layer was extracted 3 times with 100 ml of ethyl acetate/isopropanol=1/1
4. 4
   浓缩concentrated
5. 5
   其他purified on a silica gel column (30 g of silica gel, eluted with chloroform/methanol=2/1)
6. 6
   其他The corresponding fractions were collected
7. 7
   浓缩concentrated (colorless syrup, 7.47 g)

实验过程

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)

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