반응 #348441

반응 방정식

methanol

dimethylaniline

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

phosphorus pentachloride

→

2,2,2-trichloroethyl 2-bromomethyl-2-methyl-6-aminopenam-3-carboxylate hydrochloride

수율 169.9%

용매

Water

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONTo this solution were added
2. 2
   workup.STIRRINGthe solution was vigorously stirred for 30 minutes
3. 3
   기타After the reaction
4. 4
   기타precipitates
5. 5
   여과were collected by filtration
6. 6
   세척washed with methylene chloride and further with ether
7. 7
   기타dried

실험 절차

2,2,2-Trichloroethyl 2-bromomethyl-2-methyl-6-(2-phenylacetamido)penam-3-carboxylate (10.8 g) was dissolved in dried methylene chloride (300 ml). To this solution were added under cooling at -35° C. dried dimethylaniline (3.6 g) and then phosphorus pentachloride (6.4 g) and the mixture was stirred for 2.5 hours at the same temperature. To the solution was added dropwise anhydrous methanol (6.4 g) at the same temperature and the mixture was stirred for 1 hour at -15° C. Water (6.5 ml) was added to the solution and the solution was vigorously stirred for 30 minutes. After the reaction, precipitates were collected by filtration, washed with methylene chloride and further with ether and then dried to give powdery 2,2,2-trichloroethyl 2-bromomethyl-2-methyl-6-aminopenam-3-carboxylate hydrochloride (7.8 g).

출처