تفاعل #66519

ord-b52fe3e2f3204a35b4cfbbf66d690716

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe reaction mixture was quenched with water
  2. 2
    استخلاصThe aqueous phase was extracted with AcOEt
  3. 3
    غسيلThe organic phase was washed with brine
  4. 4
    تجفيفwas dried over MgSO4
  5. 5
    ترشيحwas filtered
  6. 6
    تركيزwas concentrated under reduced pressure
  7. 7
    أخرىThe crude product was used without further purification

الإجراء التجريبي

According to Scheme 3 Step 1, Method A: 2-Chloro-1-fluoro-4-nitrobenzene (1.12 mmol, 0.20 g) was added to a suspension of 3-chlorophenol (1.02 mmol, 0.10 mL), Cs2CO3 (1.25 mmol, 407 mg) in DMF/ACN (40:60, 3.6 mL). The reaction mixture was stirred at room temperature overnight. The reaction mixture was quenched with water. The aqueous phase was extracted with AcOEt. The organic phase was washed with brine, was dried over MgSO4, was filtered and was concentrated under reduced pressure. The crude product was used without further purification to obtain 2-chloro-1-(3-chlorophenoxy)-4-nitrobenzene (1.02 mmol, 288 mg, 100%) as an orange solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524726B2uspto-grants-2013_09