반응 #366853

반응 방정식

2-chloro-4-hydroxymethylpyridine

methylamine

→

4-hydroxymethyl-2-(methylamino)pyridine

수율 46.0%

용매

ethanol

반응 조건

후처리

1. 1
   기타(prepared
2. 2
   온도to cool
3. 3
   기타the mixture partitioned between saturated aqueous sodium hydrogen carbonate solution and ethyl acetate
4. 4
   기타The organic layer was separated
5. 5
   건조dried (MgSO4)
6. 6
   기타the volatiles removed by evaporation
7. 7
   기타The residue was purified by column chromatography
8. 8
   세척eluting with ethyl acetate

실험 절차

A mixture of 2-chloro-4-hydroxymethylpyridine (1.0 g, 7 mmol), (prepared as described for the starting material in Example 58), and methylamine (30 ml of a 30% solution in ethanol) was heated in a Carius tube for 16 hours at 200° C. The mixture was allowed to cool and the mixture partitioned between saturated aqueous sodium hydrogen carbonate solution and ethyl acetate. The organic layer was separated, dried (MgSO4) and the volatiles removed by evaporation. The residue was purified by column chromatography eluting with ethyl acetate to give 4-hydroxymethyl-2-(methylamino)pyridine (440 mg, 46%) as a yellow oil.

출처