反应详情

0.9 mL (0.45 mmol) Zinc(II)chloride (0.5 M solution in THF) is added dropwise to a mixture of 40.7 mg (0.15 mmol) (S)—N-{1-[4-(1-cyano-piperidin-4-yl)-phenyl]-ethyl}-acetamide (XXVII.1) and 30.6 mg (0.30 mmol N′-hydroxy-2-methylpropanimidamide in 12 mL ethylacetate. The mixture is stirred for 12 h at rt. After that the solvent is removed in vacuo and 15 mL ethanol and 2 mL conc. HCl solution are added. The mixture is refluxed for 3 h. Subsequently the mixture is concentrated, water is added and the precipitate is collected and washed with water to yield the desired product.

1. customAfter that the solvent is removed in vacuo and 15 mL ethanol and 2 mL conc. HCl solution
2. additionare added
3. temperatureThe mixture is refluxed for 3 h
4. concentrationSubsequently the mixture is concentrated
5. additionwater is added
6. customthe precipitate is collected
7. washwashed with water