تفاعل #1168923
ord-378183ca063e4b1c9eaebd4c6262b2c2
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةcooling
- 2workup.STIRRINGthe mixture was further stirred under ice-
- 3درجة الحرارةcooling for 10 minutes
- 4غسيلThe reaction mixture was washed with water
- 5استخلاصthe aqueous layer was extracted with methylene chloride (30 ml×3)
- 6تجفيفdried over anhydrous magnesium sulfate
- 7workup.DISTILLATIONAfter the solvent was distilled off
- 8أخرىthe residue was purified by column chromatography (eluent:ethyl acetate)
الإجراء التجريبي
To a solution of 5-[3-[2-(phenylamino)ethyloxy]propylthio]imidazo[1,2-a]pyridine (1.034 g, 3.158 mmoles) and triethylamine (0.88 ml, 6.3 mmoles) in methylene chloride (30 ml) was added methanesulfonyl chloride (0.37 ml, 4.7 mmoles) with stirring under ice-cooling and the mixture was further stirred under ice-cooling for 10 minutes. The reaction mixture was washed with water and the aqueous layer was extracted with methylene chloride (30 ml×3). The methylene chloride layers were combined and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent:ethyl acetate) to obtain 16 mg of the desired product (brown oily product)