تفاعل #53569

ord-dc0f6da8f3b045d2a4076930466059c1

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe resulting reaction mixture
  2. 2
    استخلاصthe organic matters were extracted with 20 ml of ethyl acetate twice
  3. 3
    غسيلwashed with 30 ml of water twice
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
  6. 6
    أخرىPurification of the residue by thin layer chromatography

الإجراء التجريبي

1.52 g (5.0 nmol) of methyl 2-chloro-4-(3-trifluoromethylpyrazolyl)benzoate, 0.66 g (8.6 mmol) of 1-propanethiol and 0.83 g (6.0 mmol) of potassium carbonate were stirred in 5 ml of N,N-dimethylformamide at 60° C. for 24 hours. The resulting reaction mixture was poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by thin layer chromatography afforded 0.31 g of methyl 2-propylthio-4-(3-trifluoromethylpyrazolyl)benzoate as a white powder (m.p. 114-116° C.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858639B2uspto-grants-2005_02