反应详情

温度

2.5 °C

To a 250 ml three necked round bottom flask was added methyl 5-aminopicolinate (2.0 g) in THF (40 ml) under nitrogen atmosphere and cooled to 0-5° C. After 15 min, 2.0 M solutions of LiAlH4 (19.7 ml) was added under nitrogen atmosphere and allow it to warm up to room temperature and stirred at same temperature for 1 hr. After completion of the reaction, the reaction mixture was cooled to 5° C. and quenched with sat. NH4Cl solution (25 ml) and diluted with water, followed by extraction with ethyl acetate. The combined organics were washed with water, dried over Na2SO4 and evaporated to afford brown oil product. The aqueous layer was concentrated to give residue which was washed with 30% methanol in ethyl acetate. Resultant washing was concentrated to afford brown oil (crude). Both the crude material were combined and subjected for column purification using 8% methanol in chloroform to yield 1.3 g of (5-aminopyridin-2-yl)methanol.

1. temperatureto warm up to room temperature
2. customAfter completion of the reaction
3. temperaturethe reaction mixture was cooled to 5° C.
4. customquenched with sat. NH4Cl solution (25 ml)
5. additiondiluted with water
6. extractionfollowed by extraction with ethyl acetate
7. washThe combined organics were washed with water
8. dry with materialdried over Na2SO4
9. customevaporated
10. customto afford brown oil product
11. concentrationThe aqueous layer was concentrated
12. customto give residue which
13. washwas washed with 30% methanol in ethyl acetate
14. washResultant washing
15. concentrationwas concentrated
16. customto afford brown oil (crude)
17. customsubjected for column purification