反应详情

[(3-tetrahydrofuryl)methyl]amine (38.0 g, 0.38 mole), 27.4 g of sodium chloride and 107.0 g of water were mixed, and the resulting mixture was cooled to −10 degree centigrade. Furthermore, 2.3 g (0.06 mole) of 96% NaOH was added to the solution and dissolved. Sodium chloride was dissolved in water with 78% of the saturated solubility at a water temperature of −10 degree centigrade. N,O-dimethyl-N′-nitroisourea (49.2 g, 0.37 mole) was introduced into the above solution, stirred at −10 degree centigrade for 4 hours, and then heated to 10 degree centigrade and further stirred for 19 hours. 35% hydrochloric acid (6.7 g, 0.07 mole) was added to the suspension so that the pH became not more than 4. Water and acetonitrile were added to the above suspension for complete dissolution. The resulting solution was analyzed by HPLC and as a result, the reaction yield of the titled compound was 95%.

1. temperaturethe resulting mixture was cooled to −10 degree centigrade
2. dissolutiondissolved
3. temperatureheated to 10 degree centigrade
4. stirringfurther stirred for 19 hours