benzhydryl (E)-(2S,3S,5R)-3-(2-chloro-vinyl)-3-methyl-4,4,7-trioxo-4-thia-1-aza-bicyclo[3.2.0]heptane-2-carboxylate → Sodium (E)-(2S,3S,5R)-3-(2-chloro-vinyl)-3-methyl-4,4,7-trioxo-4-thia-1-aza-bicyclo[3.2.0]heptane-2-carboxylate

온도

50 °C

385 mg (0.86 mmol) of benzhydryl (E)-(2S,3S,5R)-3-(2-chloro- vinyl) -3- methyl-4,4,7-trioxo-4-thia- 1-aza-bicyclo [3.2.0]heptane-2-carboxylate are dissolved in 2.3 ml of m-cresol under argon and stirred at 50° C. for 4 hours. Subsequently, the mixture was diluted with 15 ml of isobutyl methyl ketone, treated with 0.50 ml of sodium 2-ethylcaproate (2N solution in ethyl acetate) and extracted three times with 8 ml of water each time. The combined aqueous phases were washed once with 10 ml of isobutyl methyl ketone, lyophilized and the lyophilizate obtained was chromatographed over polymeric hydrophobic gel with water as the eluent. Yield: 57 mg (32%) MS: (M--Na)- 278.2 IR (KBr): 1780, 1626, 1564, 1417, 1329, 1145 cm-1

1. extractionextracted three times with 8 ml of water each time
2. washThe combined aqueous phases were washed once with 10 ml of isobutyl methyl ketone
3. customthe lyophilizate obtained
4. customwas chromatographed over polymeric hydrophobic gel with water as the eluent

ORD 기록

ord-5e606b15b4c5498c94046bd224fef880

출처 데이터셋

uspto-grants-1997_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05644053