반응 #96234

반응 방정식

t-butyl 7-benzamido-2-bromo-3-bromomethyl-3-cephem-4-carboxylate-1-oxide

→

7-benzamido-2-bromo-3-bromomethyl-3-cephem-4-carboxylic acid-1-oxide

수율 85.6%

용매

trifluoroacetic acid

반응 조건

후처리

1. 1
   기타was then evaporated to dryness under vacuo
2. 2
   workup.ADDITION25 ml of dichloromethane were added to the residue and evaporation to dryness
3. 3
   workup.ADDITIONA 1:1 mixture of ether and heptane
4. 4
   workup.ADDITIONwas added to the residue
5. 5
   여과filtered
6. 6
   세척washed with the same mixture

실험 절차

A mixture of 12.5 g of t-butyl 7-benzamido-2-bromo-3-bromomethyl-3-cephem-4-carboxylate-1-oxide and 50 ml of trifluoroacetic acid was stirred at room temperature for 15 minutes and was then evaporated to dryness under vacuo. 25 ml of dichloromethane were added to the residue and evaporation to dryness was repeated. A 1:1 mixture of ether and heptane was added to the residue and the formed crystals were vacuum filtered and washed with the same mixture to obtain 9.6 g of 7-benzamido-2-bromo-3-bromomethyl-3-cephem-4-carboxylic acid-1-oxide as an almost colorless solid, having the following characteristics:

출처