反应详情

To a mixture of 3′-amino-[1,1′-biphenyl]-3-carboxylic methyl ester (1.14 g) and N-(tert-butoxycarbonyl)glycine (0.879 g) in methylene chloride (20 mL) was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.20 g). The mixture was stirred for 3 h at room temperature, then washed twice with 1 N aqueous HCl, twice with saturated aqueous sodium bicarbonate and once with brine. The mixture was dried over sodium sulfate, filtered and concentrated to give a foam. Purification by silica gel chromatography eluting with 7:3 hexane/ethyl acetate gave 1.6 g of the title compound as a colorless oil. Electrospray MS (positive ion): (M+Na) 407.0.

1. washwashed twice with 1 N aqueous HCl, twice with saturated aqueous sodium bicarbonate and once with brine
2. dry with materialThe mixture was dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customto give a foam
6. customPurification by silica gel chromatography
7. washeluting with 7:3 hexane/ethyl acetate