HRID1392177
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of (5R,7S)-5-(4-bromobenzyl)-3-(3,5-dichlorophenyl)-7-azido-1,3-diazabicyclo[3.3.0]octane-2,4-dione (0.83 g) in acetic acid (20 mL) was added zinc powder (0.90 g). After 1 hour at room temperature, the mixture was concentrated. The residue was suspended in satd. NaHCO3 and EtOAc. The mixture was filtered and the organic layer was collected, washed with brine, dried (Na2SO4), filtered and concentrated. Purification of the residue by chromatography (silica gel: CH2Cl2: Chromatotron) afforded the titled compound (0.42 g). MS (m/z) 468 (MH+). mp 64.4° C.
WORKUP
后处理
- concentrationthe mixture was concentrated
- filtrationThe mixture was filtered
- customthe organic layer was collected
- washwashed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customPurification of the residue by chromatography (silica gel: CH2Cl2: Chromatotron)