تفاعل #2176844

معادلة التفاعل

dichloromethane

WSC

2,2-dimethylmalonic acid mono-t-butyl ester

2,2-dimethyl-1-propanol

→

2,2-dimethylmalonic acid t-butyl ester(2,2-dimethylpropyl)ester

المذيبات

water

TBME

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooling
2. 2
   workup.STIRRINGthe resulting mixture was stirred at room temperature for 2 days
3. 3
   استخلاصthe resulting mixture was extracted
4. 4
   غسيلThe organic layer was sequentially washed with water and saturated aqueous sodium chloride solution
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   ترشيحThe desiccant was filtered off
7. 7
   أخرىthe filtrate obtained
8. 8
   تركيزwas concentrated under reduced pressure
9. 9
   أخرىThe residue obtained
10. 10
    أخرىwas purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate)

الإجراء التجريبي

To a mixture of 2,2-dimethylmalonic acid mono-t-butyl ester (10 g), 2,2-dimethyl-1-propanol [CAS No. 75-84-3] (5.15 g), DMAP (1.3 g), and dichloromethane (100 mL), WSC (12.2 g) was added with stirring under ice-cooling, and the resulting mixture was stirred at room temperature for 2 days. TBME and water were added to the mixture, and the resulting mixture was extracted. The organic layer was sequentially washed with water and saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain 2,2-dimethylmalonic acid t-butyl ester(2,2-dimethylpropyl)ester (12 g).

المصدر