تفاعل #1687666

معادلة التفاعل

water

methyl gentisate

potassium carbonate

chloropropyltrimethylsilane

→

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

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةIt was cooled
2. 2
   استخلاصThe mixture was extracted with diisopropyl ether
3. 3
   غسيلThe organic phase was washed with water
4. 4
   تجفيفdried over sodium sulphate
5. 5
   تركيزconcentrated

الإجراء التجريبي

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.

المصدر