تفاعل #1880953

ord-cdff3a1fbdba4acca673281e345dd166

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled to RT
  2. 2
    استخلاصAfter extraction twice with heptane/ethyl acetate (1:1)
  3. 3
    غسيلtwice with ethyl acetate the product is washed with water and saturated sodium chloride solution
  4. 4
    تجفيفdried over MgSO4
  5. 5
    تركيزconcentrated
  6. 6
    أخرىChromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

الإجراء التجريبي

1.00 g of 2,6-difluoropyridine is introduced into 10 ml of DMF under nitrogen and 1.44 g of K2CO3 are added at RT. 1.61 g of 4-hydroxy-2-trifluoromethylthiophene are added and the mixture is heated at 80° C. for 4 h, then cooled to RT and poured into water. After extraction twice with heptane/ethyl acetate (1:1) and twice with ethyl acetate the product is washed with water and saturated sodium chloride solution, dried over MgSO4 and concentrated. Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent gives 1.7 g of 2-fluoro-6-(2-trifluoromethyl-4-thienyloxy)pyridine as a colorless oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07022650B2uspto-grants-2006_04