تفاعل #7538

معادلة التفاعل

5-[2-(3-chloropropoxy)ethyl]-1-benzothiophene

N-(3-azetidinyl)acetamide

water

ethyl acetate

→

N-(1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinyl)acetamide

المردود 37.4%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas 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=7:1)

الإجراء التجريبي

In 8 mL of N,N-dimethylformamide was dissolved 0.80 g of 5-[2-(3-chloropropoxy)ethyl]-1-benzothiophene, and 1.20 g of N-(3-azetidinyl)acetamide was added to the solution, after which the resulting mixture was stirred at 90° C. for 12 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=7:1) to obtain 0.39 g of N-(1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinyl)acetamide as a light-yellow oil.

المصدر