反应详情

3-(5-Aminopentyl)-8-naphthalen-1-ylmethyl-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one, di-trifluoroacetate (0.137 g, 0.2 mmol) prepared as described in Example 13, was dissolved in dimethylformamide (1 ml) and diisopropylethylamine (0.233 g, 1.8 mmol) and 3,5-dimethylpyrazol-1-carboxamidine nitrate (0.060 g, 0.3 mmol) was added. The mixture was stirred at room temperature for 1 h and the addition of an equal amount 3,5-dimethylpyrazol-1 carboxamidine nitrate was repeated. After stirring for 16 h the mixture was diluted with water (10 ml) and extracted with ether (5×10 ml). The aqueous phase and undissolved syrup were extracted with dichloromethane (10 ml), the dichloromethane solution was washed with water (5×10 ml), dried over MgSO4 and concentrated in vacuo, affording the title compound (0.047 g, 5.2%) as an amorphous powder.

1. stirringAfter stirring for 16 h the mixture
2. extractionextracted with ether (5×10 ml)
3. extractionThe aqueous phase and undissolved syrup were extracted with dichloromethane (10 ml)
4. washthe dichloromethane solution was washed with water (5×10 ml)
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo