تفاعل #47078

ord-679042b22ecb452c904ab20fb5acda8e

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture is cooled to RT
  2. 2
    غسيلwashed with water, brine
  3. 3
    تجفيفdried (MgSO4)
  4. 4
    ترشيحfiltered
  5. 5
    أخرىThe filtrate is evaporated
  6. 6
    أخرىthe residue purified by chromatography on silica gel
  7. 7
    غسيلelution with dichloromethane

الإجراء التجريبي

To a solution of 3-fluorophenol (560 mg, 5.0 mmol) in DMF (10 mL) is added potassium carbonate (828 mg, 6.0 mmol) followed by chloroacetonitrile (0.315 mL, 50.0 mmol). The reaction mixture is stirred and heated at 50° C. for 14 h. The reaction mixture is cooled to RT, diluted with EtOAc, and washed with water, brine, then dried (MgSO4), and filtered. The filtrate is evaporated, and the residue purified by chromatography on silica gel; elution with dichloromethane gives 712 mg of the product 386.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741493B2uspto-grants-2010_06