تفاعل #649572

ord-2422998e69df40399b86ad5c5ddb1bc7

ظروف التفاعل

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

المعالجة

  1. 1
    درجة الحرارةAfter the reaction mixture was cooled
  2. 2
    أخرىan organic layer was separated
  3. 3
    غسيلThe organic layer was successively washed with water
  4. 4
    تجفيفa saturated saline solution, and then dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONThereafter, the solvent was distilled away under a reduced pressure
  6. 6
    أخرىThe residue was purified by column chromatography (eluent; chloroform:methanol=20:1 to 10:1)

الإجراء التجريبي

1.20 g of 5-(2-(3-chloropropoxy)ethyl)-1-benzothiophene was dissolved in 12 ml of N,N-dimethylformamide. Thereafter, 0.82 g of 3-pyrrolidinol and 1.30 g of potassium carbonate were added to the obtained solution, and the mixture was then stirred at 85° C. for 2.5 hours. After the reaction mixture was cooled, water and ethyl acetate were added thereto, and an organic layer was separated. The organic layer was successively washed with water and a saturated saline solution, and then dried over anhydrous magnesium sulfate. Thereafter, the solvent was distilled away under a reduced pressure. The residue was purified by column chromatography (eluent; chloroform:methanol=20:1 to 10:1), so as to obtain 0.78 g of an achromatic oil product, 1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-3-pyrrolidinol.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08067406B2uspto-grants-2011_11