反应详情

温度

10 °C

3.15 ml of methanolic methylamine solution (containing 33.6% by weight, i.e. 0.024 moles, of methylamine) are added to a solution of 1.3 g (0.004 moles) of 2,6-bis(chloromethyloxy-carbonyloxymethyl)pyridine (prepared as described in Example 1) at about 0° C. under cooling at such a rate that the temperature is maintained at 10° C. or lower. A crystalline precipitate is separated. After completing the addition, 5 ml of water are added to the mixture which is then cooled to 2° to 5° C. The precipitate is separated by filtration and dried to give 0.97 g of the title compound, m.p.: 132°-135° C. The yield is 97% as calculated for 2,6-bis(hydroxymethyl)pyridine. The 2,6-bis(hydroxymethyl)pyridine bis(N-methylcarbamate) content of the thus-obtained product is 98% based on the spectrophotometric determination.

1. temperatureunder cooling at such a rate that the temperature
2. customA crystalline precipitate is separated
3. additionthe addition, 5 ml of water
4. additionare added to the mixture which
5. temperatureis then cooled to 2° to 5° C
6. customThe precipitate is separated by filtration
7. customdried