반응 #63262

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methylamine

2,6-bis(chloromethyloxy-carbonyloxymethyl)pyridine

→

title compound

수율 97.0%

2,6-bis(hydroxymethyl)pyridine bis(N-methylcarbamate)

수율 97.0%

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후처리

1. 1
   온도under cooling at such a rate that the temperature
2. 2
   기타A crystalline precipitate is separated
3. 3
   workup.ADDITIONthe addition, 5 ml of water
4. 4
   workup.ADDITIONare added to the mixture which
5. 5
   온도is then cooled to 2° to 5° C
6. 6
   기타The precipitate is separated by filtration
7. 7
   기타dried

실험 절차

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.

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