반응 #96175
ord-6a0e11892b014bdcbc21695dc4dabf20
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과The DCC-urea was filtered
- 2세척washed with CH2Cl2
- 3세척The filtrate was then washed 2×125 ml 1N HCl, 2×125 ml saturated NaHCO3, 2×125 ml brine
- 4건조dried (MgSO4)
- 5여과filtered
- 6농축concentrated
실험 절차
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.