تفاعل #2348089

ord-4ecf643ab25c4906a12ec5cd57602a18

معادلة التفاعل

OO
hydrogen peroxide
Cc1cc(F)c(F)c(OB(O)O)c1
compound ( 3 )
Cc1cc(F)c(F)c(OB(O)O)c1
2,3-difluoro-5-methylphenylboric acid
Cc1cc(O)c(F)c(F)c1
2,3-difluoro-5-methylphenol

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةUnder cooling with an ice bath
  2. 2
    workup.DISSOLUTIONhaving been dissolved in 300 mL
  3. 3
    درجة الحرارةUnder cooling with an ice bath
  4. 4
    أخرىto terminate
  5. 5
    أخرىthe reaction
  6. 6
    استخلاصThe aqueous layer was extracted with diethyl ether, which
  7. 7
    workup.ADDITIONwas added to the organic layer
  8. 8
    غسيلthe organic layer was washed with a saturated sodium hydrogensulfite aqueous solution
  9. 9
    تجفيفa saturated saline and then dried over anhydrous magnesium sulfate
  10. 10
    workup.DISTILLATIONThe solvent was distilled off in vacuo

الإجراء التجريبي

Under cooling with an ice bath, 53.1 g of aqueous hydrogen peroxide was slowly added dropwise to the compound (3) having been dissolved in 300 mL, followed by stirring at room temperature for 3 hours. Under cooling with an ice bath, 100 mL of a saturated sodium hydrogensulfite aqueous solution was added dropwise thereto to terminate the reaction. The aqueous layer was extracted with diethyl ether, which was added to the organic layer, and the organic layer was washed with a saturated sodium hydrogensulfite aqueous solution and a saturated saline and then dried over anhydrous magnesium sulfate. The solvent was distilled off in vacuo to obtain 22.7 g of 2,3-difluoro-5-methylphenol (4).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07846513B2uspto-grants-2010_12