تفاعل #649567

ord-d06c4b5c118a48db8753c609d92c963b

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  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=7:1)

الإجراء التجريبي

0.80 g of 5-(2-(3-chloropropoxy)ethyl)-1-benzothiophene was dissolved in 8 ml of N,N-dimethylformamide. Thereafter, 1.20 g of N-(3-azetidinyl)acetamide was added to the obtained solution, and the obtained mixture was stirred at 90° C. for 12 hours. After cooling, water and ethyl acetate were added to the reaction mixture, 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=7:1), so as to obtain 0.39 g of a light yellow oil product, N-(1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-3-azetidinyl)acetamide.

المصدر

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