تفاعل #1557824

معادلة التفاعل

terphthalic acid monomethyl ester

3-hydroxy-butane-2-one

pyridine

EDCl

HCl

→

title compound

Terephthalic acid 1-methyl ester 4-(1-methyl-2-oxo-propyl) ester

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONThe reaction mixture was poured into ice cold water
2. 2
   استخلاصextracted with ethyl acetate (100 mL×2)
3. 3
   غسيلThe combined organic layers were washed with water (50 mL×2) and with brine
4. 4
   تجفيفdried over anhydrous sodium sulphate
5. 5
   تركيزconcentrated
6. 6
   أخرىthe obtained residue was purified by column chromatography

الإجراء التجريبي

A mixture of terphthalic acid monomethyl ester (1.0 g, 5 mmol), 3-hydroxy-butane-2-one (0.531 g, 6.8 mmol), 4-dimethylamino pyridine (1.27 g, 10 mmol), pyridine (0.79 g, 10 mmol) and EDCl.HCl (1.6 g, 8 mmol) was stirred in dry DMF (10 mL) over night under nitrogen atmosphere. The reaction mixture was poured into ice cold water and extracted with ethyl acetate (100 mL×2). The combined organic layers were washed with water (50 mL×2) and with brine, then dried over anhydrous sodium sulphate and concentrated. the obtained residue was purified by column chromatography using 3% ethyl acetate in hexane to obtain the title compound.

المصدر