تفاعل #1382788

ord-39b831b2ad3a4bbb9bfb2aebc10b0e6d

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    درجة الحرارةis refluxed for 30 minutes
  3. 3
    أخرىThe aqueous phase is separated off
  4. 4
    استخلاصextracted with diethyl ether
  5. 5
    تجفيفdried with sodium sulphate
  6. 6
    أخرىevaporated down
  7. 7
    أخرىThe residue is chromatographed on a silica gel column (petroleum ether/ethyl acetate=9:1)

الإجراء التجريبي

A Grignard is prepared from 1.77 g (73 mmol) of iodine-activated magnesium and 18.70 g (72 mmol) 1-bromo-4-chloro-2-trifluoromethyl-benzene dissolved in 150 mL diethyl ether. 5.46 g (72 mmol) isobutyraldehyde in 30 mL diethyl ether are added dropwise to the Grignard reagent at ambient temperature. After the addition has ended the reaction mixture is refluxed for 30 minutes and then stirred overnight at ambient temperature. It is combined with ice water and acidified with hydrochloric acid. The aqueous phase is separated off and extracted with diethyl ether. The organic phases are combined, dried with sodium sulphate and evaporated down. The residue is chromatographed on a silica gel column (petroleum ether/ethyl acetate=9:1). 10.5 g of oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07244728B2uspto-grants-2007_07