反应详情

温度

120 °C

(2.00 g, 8.76 mmol), 4-chloropyridine hydrochloride (1.31 g, 8.76 mmol) and TEA (2.44 ml, 17.55 mmol) were in i-PrOH (10 ml) and heated in the microwave for 2 h at 120° C. The solvent was removed under vacuum. The product was purified by column chromatography (silica gel, DCM/(7 M NH3 in MeOH, 99:1→98:2→95:5). 2. The reaction was performed under an argon atmosphere. The amine from stage 1 (1.87 g, 4.56 mmol) was dissolved in dry THF (75 ml) and cooled to 0° C. A solution of LAH (2.4 M in THF, 7.6 ml, 18.25 mmol) was added dropwise. On completion of the addition the mixture was heated to 60° C. After a reaction time of 4.5 h the mixture was cooled to RT and stirred overnight at RT. Na2SO4.10H2O was added to the reaction solution until no further H2 evolution could be detected. The viscous solution was dried by adding Na2SO4 and filtered after approximately 30 min. The residue was rewashed with THF. The combined filtrates were concentrated to dryness and the crude product obtained was purified by column chromatography.

1. customThe solvent was removed under vacuum
2. customThe product was purified by column chromatography (silica gel, DCM/(7 M NH3 in MeOH, 99:1→98:2→95:5)
3. temperaturecooled to 0° C
4. additionOn completion of the addition the mixture
5. temperaturewas heated to 60° C
6. temperatureAfter a reaction time of 4.5 h the mixture was cooled to RT
7. customThe viscous solution was dried
8. additionby adding Na2SO4
9. filtrationfiltered after approximately 30 min
10. concentrationThe combined filtrates were concentrated to dryness