反应详情

Under nitrogen, 0.38 g (1.1 mmol) of 3-(2,2-diethoxyethyl)amino-2-methyl-4-(methyl-sulfonyl)benzoic acid, 0.16 g (1.4 mmol) of 5-hydroxy-1-methylpyrazole and 0.25 g (1.3 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were dissolved in dry CH3CN. The mixture was stirred at RT for 1 day and allowed to stand for 2 days. 0.31 ml (2.2 mmol) of NEt3, 0.06 ml (0.4 mmol) of Me3SiCN and a spatula tip of KCN were added, and the mixture was stirred at RT for 2 days. The solvent was removed under reduced pressure, and the residue was taken up in CH2Cl2 and 10% strength H2SO4. The organic phase was removed and dried over MgSO4, and the solvent was removed under reduced pressure. The residue were purified by preparative HPLC. This gave 0.14 g of a red oil in a purity of 93%.

1. waitto stand for 2 days
2. stirringthe mixture was stirred at RT for 2 days
3. customThe solvent was removed under reduced pressure
4. customThe organic phase was removed
5. dry with materialdried over MgSO4
6. customthe solvent was removed under reduced pressure
7. customThe residue were purified by preparative HPLC