تفاعل #2348098

معادلة التفاعل

compound ( 10 )

2,3-difluoro-4-ethoxy-6-methylphenylboric acid

hydrogen peroxide

sodium

→

2,3-difluoro-5-methylphenol

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةUnder cooling with an ice bath
2. 2
   درجة الحرارةUnder cooling with an ice bath
3. 3
   أخرىto terminate
4. 4
   أخرىthe reaction
5. 5
   استخلاصan aqueous layer was extracted with diethyl ether, which
6. 6
   workup.ADDITIONwas added to the organic layer
7. 7
   غسيلThe organic layer was washed with a saturated sodium hydrogensufite aqueous solution and saturated saline
8. 8
   تجفيفdried over anhydrous magnesium sulfate
9. 9
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

الإجراء التجريبي

Under cooling with an ice bath, 6.57 g of aqueous hydrogen peroxide was slowly added dropwise to the compound (10) having been dissolved in 37 mL of THF, followed by stirring at room temperature for 3 hours. Under cooling with an ice bath, 20 mL of a saturated sodium hydrogensufite aqueous solution was added thereto to terminate the reaction, and an aqueous layer was extracted with diethyl ether, which was added to the organic layer. The organic layer was washed with a saturated sodium hydrogensufite aqueous solution and saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 3.84 g of 2,3-difluoro-5-methylphenol (11).

المصدر