تفاعل #1576028

معادلة التفاعل

sodium hydrogencarbonate

(Z)-1-(3-amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-ethene

Fmoc-Gly

BOP reagent

→

final product

المردود 43.5%

(Z)-1-(3-Amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-ethene Fmoc-glycineamide

المردود 43.5%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter the reaction mixture was cooled
2. 2
   استخلاصThe resulting mixture was extracted three times with dichloromethane
3. 3
   تجفيفThe extract was dried over anhydrous sodium sulfate
4. 4
   تركيزconcentrated to dryness under reduced pressure
5. 5
   أخرىThe product was purified through silica-gel column chromatography (
6. 6
   workup.ADDITIONmixture of ethyl acetate and hexane at a ratio by volume of 1:2)

الإجراء التجريبي

Two grams (6.3 mmols) of (Z)-1-(3-amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-ethene, 2.3 g of Fmoc-Gly and 11 g (25 mmols) of a BOP reagent were dissolved in 40 ml of N,N-dimethylformamide, and the mixture was heated at 60° C. for 2 hours. After the reaction mixture was cooled, a saturated aqueous solution of sodium hydrogencarbonate was added thereto. The resulting mixture was extracted three times with dichloromethane. The extract was dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure. The product was purified through silica-gel column chromatography (mixture of ethyl acetate and hexane at a ratio by volume of 1:2) to give 1.63 of the final product in a yield of 43.5%.

المصدر