反应详情

To a solution of the compound of example 29 (200 mg, 0.41 mmol) and HOBt (66 mg, 0.49 mmol) in DMF (2 mL), were added 4-biphenylethylamine (124 mg, 0.62 mmol) and DIC (78 μL) respectively. The reaction mixture was stirred for 24 h at room temperature. The reaction mixture was partitioned between HCl (0.5N, excess) and ethyl acetate. The aqueous phase was extracted several times with ethyl acetate. The recombined organic layer was washed with brine, with a saturated sodium hydrogen carbonate solution, and again with brine. The solvent was evaporated following drying over sodium sulfate, and the crude was flashed using 30% ethyl acetate in hexanes. 1H-NMR (CDCl3, 400 MH: 1.55(s, 9H); 1.41–1.57(m, 2H); 2.04–2.28(m, 6H); 2.54(m, 1H); 2.80(m, 2H); 3.45–3.55(m, 2H), 5.66(m, 1H); 7.19–7.57(m, 24H).

1. customThe reaction mixture was partitioned between HCl (0.5N, excess) and ethyl acetate
2. extractionThe aqueous phase was extracted several times with ethyl acetate
3. washThe recombined organic layer was washed with brine, with a saturated sodium hydrogen carbonate solution
4. customThe solvent was evaporated
5. dry with materialfollowing drying over sodium sulfate