反应详情

To the solution of 877 mg (3.41 mmol) of the compound prepared in (a) (3.41 mmole) in the mixture of 6.8 ml of dimethylformamide and 1.4 ml of pyridine were added 874 mg of N,N'-disuccinimidyl carbonate and a catalytic amount of 4-dimethylaminopyridine, and the resulting mixture was stirred at room temperature for 3 hours, whereafter 1.45 g of the compound prepared in (b) and 0.59 ml of N,N-diisopropylethylamine were added. The mixture was further stirred at room temperature overnight. After the reaction mixture was concentrated under reduced pressure, the resulting solid product was purified by column chromatography on silica gel. The solid product thus obtained was washed with ether to give 1.1 g of dimethyl [[4-[[[trans-4-(t-butyloxycarbonylaminomethyl)cyclohexyl]carbonylamino]acetyl]-o-phenylene]dioxy]diacetate as pale yellow crystals (yield, 59%).

1. additionwere added
2. concentrationAfter the reaction mixture was concentrated under reduced pressure
3. customthe resulting solid product was purified by column chromatography on silica gel
4. customThe solid product thus obtained
5. washwas washed with ether
6. customto give