تفاعل #1365538

معادلة التفاعل

p-nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-hydroxy-3-cephem-4-carboxylate

N-(2-chloro-1,1,2-trifluoroethyl) diethylamine

→

7-[2-(2-Thienyl)acetamido]-3-fluoro-3-cephem-4-carboxylic acid

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was heated for 30 minutes
2. 2
   درجة الحرارةunder gentle reflux
3. 3
   أخرىwas then evaporated to dryness in vacuo
4. 4
   workup.DISSOLUTIONthe residue was dissolved in a mixture of ethyl acetate-water
5. 5
   أخرىthe organic layer was separated
6. 6
   غسيلThe organic layer was washed with 5% hydrochloric acid, water and brine
7. 7
   أخرىwas then dried
8. 8
   أخرىThe dried reaction product solution
9. 9
   تركيزwas concentrated to a small volume and n-hexane
10. 10
    workup.ADDITIONwas added
11. 11
    أخرىto precipitate

الإجراء التجريبي

To a solution of 325 mg. (0.7 mmole) of p-nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-hydroxy-3-cephem-4-carboxylate in 10 ml. of methylene chloride was slowly added an equivalent amount of N-(2-chloro-1,1,2-trifluoroethyl) diethylamine. The reaction mixture was heated for 30 minutes under gentle reflux and was then evaporated to dryness in vacuo. the residue was dissolved in a mixture of ethyl acetate-water and the organic layer was separated. The organic layer was washed with 5% hydrochloric acid, water and brine and was then dried. The dried reaction product solution was concentrated to a small volume and n-hexane was added to precipitate, p-nitrobenzyl 7-[2-(2-thienyl)acetamido]-3-fluoro-3-cephem-4-carboxylate.

المصدر