반응 #167822

반응 방정식

6-tetrazol-1-yl-pyridin-3-ol

Potassium carbonate

potassium iodide

propargyl chloride

→

5-(Prop-2-ynyloxy)-2-(1H-tetrazol-1-yl)pyridine

용매

N,N-dimethylformamide

water

반응 조건

후처리

1. 1
   기타To a flask under N2 fitted with a reflux condenser
2. 2
   온도The reaction was cooled to room temperature
3. 3
   기타precipitation
4. 4
   여과The solid was filtered off
5. 5
   세척washed with water
6. 6
   기타dried overnight
7. 7
   기타The expected product was used in the next step without further purification

실험 절차

To a flask under N2 fitted with a reflux condenser was added 6-tetrazol-1-yl-pyridin-3-ol (2.25 g, 13.7 mmol) and N,N-dimethylformamide (8.2 mL). Potassium carbonate (3.79 g, 27.4 mmol, 2 eq.), potassium iodide (0.143 g, 0.86 mmol, 0.06 eq.) and propargyl chloride (1.98 mL, 17.9 mmol, 1.3 eq.) were added and heated at 80° C. for three hours. The reaction was cooled to room temperature and 10 mL of water was added to affect precipitation. The solid was filtered off, washed with water and dried overnight. The expected product was used in the next step without further purification. 1H NMR (DMSO-d6): δ 10.08 (1H, s), 8.36 (1H, d, J=3.0 Hz), 8.01 (1H, d, J=9 Hz), 7.79 (1H, dd, J=3.0, 9.0 Hz), 5.01 (2H, s), 3.71 (1H, s)

출처