反应 #1687666

反应方程式

water

methyl gentisate

potassium carbonate

chloropropyltrimethylsilane

→

methyl 2-hydroxy-5-(3-trimethylsilanylpropyloxy)benzoate

溶剂

DMF

反应条件

后处理

1. 1
   温度It was cooled
2. 2
   萃取The mixture was extracted with diisopropyl ether
3. 3
   洗涤The organic phase was washed with water
4. 4
   干燥dried over sodium sulphate
5. 5
   浓缩concentrated

实验过程

To a mixture of methyl gentisate (16.8 g, 0.1 mol) and potassium carbonate (15.2 g, 0.11 mol) in 80 ml of DMF, under a nitrogen atmosphere at 80° C., was added chloropropyltrimethylsilane (16.6 g, 0.11 mol) dropwise over 20 minutes. The mixture was heated at 90° C. for 8 hours. It was cooled and poured into 200 ml of water. The mixture was extracted with diisopropyl ether. The organic phase was washed with water, dried over sodium sulphate and then concentrated. After chromatography on silica of the yellow oil obtained (eluent: 90/10 heptane/CH2Cl2), 3.3 g of a clean fraction of methyl 2-hydroxy-5-(3-trimethylsilanylpropyloxy)benzoate were recovered.

来源