تفاعل #2463441

معادلة التفاعل

sulfuric acid

hydroxy(4-isopropylphenyl)acetic acid

2,3,5-trimethylphenol

→

title compound

المردود 65.0%

3-(4-Isopropylphenyl)-4,6,7-trimethyl-1-benzofuran-2 (3H)-one

المردود 65.0%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصwas extracted with diisopropyl ether
2. 2
   غسيلThe extract was washed with water
3. 3
   تجفيفa saturated sodium hydrogen carbonate solution, and then was dried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
5. 5
   أخرىto obtain a residue, which
6. 6
   أخرىwas purified by silica gel column chromatography (hexane ethyl acetate=8:1)

الإجراء التجريبي

To a mixture of hydroxy(4-isopropylphenyl)acetic acid synthesized in Reference Example 1 (11.8 g, 60.8 mmol) and 2,3,5-trimethylphenol (12.4 g, 91.2 mmol) was added 70% sulfuric acid (10 mL) at room temperature, and the mixture was stirred at 115° C. for 12 hours. The mixture was added to water and was extracted with diisopropyl ether. The extract was washed with water and a saturated sodium hydrogen carbonate solution, and then was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain a residue, which was purified by silica gel column chromatography (hexane ethyl acetate=8:1) to obtain 10.9 g (yield 65%) of the title compound. Melting point: 107-108° C. (hexane-ethyl acetate).

المصدر