تفاعل #1874271

معادلة التفاعل

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

methyl iodide

sodium hydride

Water

→

title compound

المردود 94.0%

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

المردود 94.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىat 0° C.
2. 2
   workup.STIRRINGthe mixture was stirred for at room temperature 30 minutes
3. 3
   استخلاصthe product was extracted with ethyl acetate
4. 4
   استخلاصThe combined extract
5. 5
   غسيلwas washed with water
6. 6
   تجفيفdried over magnesium sulfate
7. 7
   تركيزconcentrated under reduced pressure
8. 8
   أخرىto obtain the residue, which
9. 9
   أخرىwas purified by silica gel column chromatography (hexane:ethyl acetate=4:1)

الإجراء التجريبي

To a solution of 3-(4-isopropylphenyl)-4,6,7-trimethyl-1-benzofuran-2(3H)-one synthesized in Reference Example 2 (2.10 g, 7.13 mmol) in DMF (30 mL) was added sodium hydride (a 60% fluidized paraffin dispersion, 314 mg, 7.84 mmol) at 0° C., and the mixture was stirred at room temperature for 30 minutes. To the reaction solution was added methyl iodide (1.11 g, 7.84 mmol) and the mixture was stirred for at room temperature 30 minutes. Water was added to the reaction solution and the product was extracted with ethyl acetate. The combined extract was washed with water, dried over magnesium sulfate and then concentrated under reduced pressure to obtain the residue, which was purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to obtain 2.07 g (yield 94%) of the title compound as an oily matter.

المصدر