反应详情

2-Acetylthio-3-chlorobenzoic acid (11.5 g, 50 mmol) and N-cyclopentylglycine t-butyl ester (10.0 g, 50 mmol) in methylene chloride (350 ml) were cooled to 0°-5° C., and N,N1 -dicyclohexylcarbodiimide (10.3 g, 50 mmol) in methylene chloride (50 ml) was added. The mixture was stirred overnight. The DCC-urea was filtered and washed with CH2Cl2. The filtrate was then washed 2×125 ml 1N HCl, 2×125 ml saturated NaHCO3, 2×125 ml brine, dried (MgSO4), filtered and concentrated to give 20.6 g of an oil. The crude product was used without further purification in the next step.

1. filtrationThe DCC-urea was filtered
2. washwashed with CH2Cl2
3. washThe filtrate was then washed 2×125 ml 1N HCl, 2×125 ml saturated NaHCO3, 2×125 ml brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated