反应详情

A solution of 5-azaindole (1.19 g, 10.0 mmol), dimethylamine hydrochloride (0.98 g, 12.0 mmol) and paraformaldehyde (0.36 g, 12.0 mmol-equivalents) in 1-butanol is heated at reflux temperature for 5 h and concentrated in vacuo. The concentrate is diluted with saturated aqueous NaHCO3 and extracted with 4:1 CH2Cl2:ethanol. The combined extracts are dried over MgSO4, concentrated in vacuo and filtered. The filtercake is air-dried to afford the title compound as a yellow solid, 0.680 g (39% yield), identified by NMR analysis.

1. temperatureat reflux temperature for 5 h
2. concentrationconcentrated in vacuo
3. additionThe concentrate is diluted with saturated aqueous NaHCO3
4. extractionextracted with 4:1 CH2Cl2
5. dry with materialThe combined extracts are dried over MgSO4
6. concentrationconcentrated in vacuo
7. filtrationfiltered
8. customThe filtercake is air-dried