반응 #930461

반응 방정식

water

methyl gentisate

potassium carbonate

chloropropyl trimethyl silane

→

methyl 2-hydroxy-4-(3-trimethylsilanyl-propyloxy)-benzoate

용매

DMF

반응 조건

후처리

1. 1
   온도It is cooled
2. 2
   추출Extraction
3. 3
   세척The organic phase is washed with water
4. 4
   건조dried with sodium sulfate
5. 5
   농축concentrated

실험 절차

To a mixture of methyl gentisate (16.8 g, 0.1 mole) and potassium carbonate (15.2 g, 0.11 mole) in 80 ml of DMF in a nitrogen atmosphere at 80° C. is added chloropropyl trimethyl silane (16.6 g, 0.11 mole) drop by drop over a 20-minute period. The mixture is heated to 90° C. for 8 hours. It is cooled and then poured into 200 ml of water. Extraction is performed with diisopropyl ether. The organic phase is washed with water, dried with sodium sulfate, and then concentrated. After silica chromatography of the resulting yellow oil (eluent: Heptane/CH2Cl2 90:10) we obtain 3.3 g of a clean fraction of methyl 2-hydroxy-4-(3-trimethylsilanyl-propyloxy)-benzoate.

출처