반응 #348434

반응 방정식

2,2,2-Trichloroethyl 2-bromomethyl-2-methyl-6-(2-phenylacetamido)-penam-3-carboxylate

methanol

→

2,2,2-trichloroethyl 2-methoxymethyl-2-methyl-6-(2-phenylacetamido)penam-3-carboxylate

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred for 2 hours at the same temperature
2. 2
   여과the reaction mixture was filtered
3. 3
   세척the filtrate was washed with sodium bicarbonate aqueous solution
4. 4
   건조with water, dried over magnesium sulfate
5. 5
   농축concentrated
6. 6
   세척eluted with chloroform
7. 7
   기타The eluate was separated into fractions of about 20 ml
8. 8
   기타the first and second fractions were collected
9. 9
   workup.DISTILLATIONAfter distilling off the solvent
10. 10
    기타the residue was dried

실험 절차

2,2,2-Trichloroethyl 2-bromomethyl-2-methyl-6-(2-phenylacetamido)-penam-3-carboxylate (1.10 g) was dissolved in methylene chloride (12 ml) and to this solution was added methanol (3 ml). And to the solution was added silver fluoroborate (0.45 g) under stirring under cooling at -10° C. and the mixture was stirred for 2 hours at the same temperature. After the reaction was completed, the reaction mixture was filtered and the filtrate was washed with sodium bicarbonate aqueous solution and then with water, dried over magnesium sulfate and thereafter concentrated. The residue was subjected to column chromatography on silica gel (25 g) and eluted with chloroform. The eluate was separated into fractions of about 20 ml and the first and second fractions were collected. After distilling off the solvent, the residue was dried to give oily 2,2,2-trichloroethyl 2-methoxymethyl-2-methyl-6-(2-phenylacetamido)penam-3-carboxylate.

출처