반응 #947885
ord-e6c85256c5b54ec58b2b7c98de08a5f5
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타The resulting reaction mixture
- 2여과The urea was filtered off
- 3기타the product was transferred to a separatory funnel
- 4세척washed with 1N HCl (10 mL), water (30 mL) and brine (30 mL)
- 5여과The product was filtered
- 6건조after drying over MgSO4
- 7기타the solvent was evaporated
- 8기타to leave a residue
- 9기타The product obtained in >95% yield
실험 절차
To a solution of cholesterol (2.0 g, 5.17 mM) in methylene chloride (20 mL) was added 5-hexenoic acid (0.68 mL, 5.69 mM) followed by the addition of DCC (1.60 g, 7.76 mM) and 4-PP (0.115 g, 0.78 mM) under nitrogen atmosphere. The resulting reaction mixture was stirred at ambient temperature for 1 h and worked up with the addition of methyl t-butyl ether (60 mL). The urea was filtered off, and the product was transferred to a separatory funnel, washed with 1N HCl (10 mL), water (30 mL) and brine (30 mL). The product was filtered after drying over MgSO4 and the solvent was evaporated to leave a residue. The product obtained in >95% yield was characterized by 1H NMR.