反应详情

Under nitrogen, 0.43 g (1.5 mmol) of 3-isobutylamino-2-methyl-4-(methyl-sulfonyl)benzoic acid, 0.22 g (2.0 mmol) of 1-ethyl-5-hydroxypyrazole and 0.35 g (1.8 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were dissolved in dry acetonitrile. The mixture was stirred at RT for 1 day and allowed to stand for 2 days. 0.42 ml (3.0 mmol) of NEt3, 0.08 ml (0.6 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, and the residue was taken up in CH2Cl2 and 10% strength H2SO4. The organic phase was separated off and dried over MgSO4, and the solvent was removed under reduced pressure. The residue was crystallized from acetonitrile. This gave 0.16 g of a red solid of a purity of 96%.

1. waitto stand for 2 days
2. stirringthe mixture was stirred at RT for 2 days
3. customThe solvent was removed
4. customThe organic phase was separated off
5. dry with materialdried over MgSO4
6. customthe solvent was removed under reduced pressure
7. customThe residue was crystallized from acetonitrile