تفاعل #2464339

ord-00ab880a920c4cc98bafb2f73b92c8a6

ظروف التفاعل

درجة الحرارة
85°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added to the solution
  2. 2
    درجة الحرارةAfter the reaction mixture was cooled
  3. 3
    أخرىthe organic layer was separated
  4. 4
    غسيلThe organic layer was washed with water
  5. 5
    تجفيفa saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONdistilled under reduced pressure
  7. 7
    أخرىto remove the solvent
  8. 8
    أخرىThe residue was purified by a column chromatography (eluent; chloroform : methanol 20:1 to 10:1)

الإجراء التجريبي

In 12 mL of N,N-dimethylformamide was dissolved 1.20 g of 5-[2-(3-chloropropoxy)ethyl]-1-benzothiophene, and 0.82 g of 3-pyrrolidinol and 1.30 g of potassium carbonate were added to the solution, after which the resulting mixture was stirred at 85° C. for 2.5 hours. After the reaction mixture was cooled, water and ethyl acetate were added thereto and the organic layer was separated. The organic layer was washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent. The residue was purified by a column chromatography (eluent; chloroform : methanol 20:1 to 10:1) to obtain 0.78 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinol as a colorless oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07468443B2uspto-grants-2008_12