تفاعل #5136

معادلة التفاعل

methyl 11-chloroacetamido-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate

imidazole

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product

Methyl 11-(1-imidazolyl)acetamido-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto cool
2. 2
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
3. 3
   استخلاصThe obtained residue was extracted with 300 ml of methylene chloride
4. 4
   غسيلThe extract was washed successively with saturated sodium bicarbonate aqueous solution and saturated sodium chloride aqueous solution
5. 5
   تجفيفAfter drying over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
7. 7
   غسيلThe resulting residue was subjected to silica gel column chromatography (eluting solvent; chlororform:methanol=10:1)

الإجراء التجريبي

Crude methyl 11-chloroacetamido-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate, 3.0 g, was heated to reflux for 4 hours in 100 ml of toluene together with 0.9 g of imidazole. After allowing to cool, the solvent was distilled off under reduced pressure. The obtained residue was extracted with 300 ml of methylene chloride. The extract was washed successively with saturated sodium bicarbonate aqueous solution and saturated sodium chloride aqueous solution. After drying over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was subjected to silica gel column chromatography (eluting solvent; chlororform:methanol=10:1) to give 1.6 g of the product.

المصدر