反应详情

To a stirred solution of S-benzyl-N-(3-benzylthio-2,2-dimethylpropionyl)-L-cysteine (2.04 g) and N-hydroxysuccinimide (0.563 g) in DMF (5 ml), DCC (1.11 g) dissolved in DMF (5 ml) was added dropwise. The mixture was stirred for 0.5 hr. under ice cooling and for 0.5 hr. at room temperature, and filtered. To the filtrate, 1,3-diaminopropane (1.09 g) dissolved in DMF (30 ml) was added dropwise with stirring. The mixture was stirred for lhr and water was added to the mixture, and then the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The oily residue was purified by a silica gel column chromatography to give 1.6 g (69%) of the titled compound.

1. additionwas added dropwise
2. waitunder ice cooling and for 0.5 hr
3. filtrationat room temperature, and filtered
4. dissolutionTo the filtrate, 1,3-diaminopropane (1.09 g) dissolved in DMF (30 ml)
5. additionwas added dropwise
6. stirringwith stirring
7. stirringThe mixture was stirred for lhr and water
8. additionwas added to the mixture
9. extractionthe mixture was extracted with ethyl acetate
10. washThe organic layer was washed with water and saturated sodium chloride
11. dry with materialdried over anhydrous magnesium sulfate
12. concentrationconcentrated in vacuo
13. customThe oily residue was purified by a silica gel column chromatography