反应详情

0.301 g (1 mmol) of (3R)-4-(4-toluenesulfonyl)thiomorpholine-3-carboxylic acid, 0.215 g (1.1 mmol) of L-leucine ethyl ester hydrochlorid, 0.227 g (1.2 mmol) of DCC and 0.122 g (1 mmol) of DMAP were dissolved in 30 mL of CH2Cl2, 0.2 ml (1.4 mmol) of TEA was added. The mixture was stirred for 24 h at room temperature. The solid was filtrated and the solvent was evaporated. The residual was dissolved in a suitable amount of ethyl acetate (20 ml) and then the mixture was filtered to remove insoluble substance. The ethyl acetate was added to 60 ml and then the liquid was washed with 10% NaHCO3 solution, saturated NaCl solution and dried over Na2SO4. After the drying agent was removed and part of ethyl acetate was evaporated, the crude product was purified by flash column chromatography (eluent: CH2Cl2:CH3Cl=1:1) to obtain the product as a oil (0.36 g).

1. filtrationThe solid was filtrated
2. customthe solvent was evaporated
3. dissolutionThe residual was dissolved in a suitable amount of ethyl acetate (20 ml)
4. filtrationthe mixture was filtered
5. customto remove insoluble substance
6. additionThe ethyl acetate was added to 60 ml
7. washthe liquid was washed with 10% NaHCO3 solution, saturated NaCl solution
8. dry with materialdried over Na2SO4
9. customAfter the drying agent was removed
10. custompart of ethyl acetate was evaporated
11. customthe crude product was purified by flash column chromatography (eluent: CH2Cl2:CH3Cl=1:1)