反应详情

6-[acetoxy-(5-ethoxy-7,8-dihydro-6H-3,4,8b-triaza-as-indacen-2-yl)-methyl]-6-bromo-7-oxo-4-thia-1-aza-bicyclo[3.2.0]hept-2-ene-2-carboxylic acid 4-nitro-benzyl ester (1.03 gram, 1.565 mmol) was suspended in 20 ml THF and 20 ml pH=6.5 aqueous phosphate buffer. The mixture was then subjected to 45 psi hydrogen for two hours. Then it was filtered through a pad of celite and concentrated in vacuo to remove most of the THF. The solution was then cooled to zero degree and basified to pH=8 with 1 N sodium hydroxide. Then it was purified via reverse phase HPLC using 1 liter of water followed by 5%˜25% acetonitrile and water. Water was then removed through concentrate in vacuo and 100 mg of product was collected.

1. filtrationThen it was filtered through a pad of celite
2. concentrationconcentrated in vacuo
3. customto remove most of the THF
4. temperatureThe solution was then cooled to zero degree and basified to pH=8 with 1 N sodium hydroxide
5. customThen it was purified via reverse phase
6. customWater was then removed
7. concentrationthrough concentrate in vacuo and 100 mg of product
8. customwas collected