反应详情

温度

70 °C

3-Fluoro-5-(4-methanesulfonyl-phenoxy)-benzonitrile (22.31 mmol; 6.50 g) was dissolved in dry DMF (32.5 ml) and this was added to the flask containing the anion of S-1-methoxyproapan-2-ol. The mixture was heated to 70° C. and held at 70° C. for 18 hrs. Water (20 ml) was added, then sufficient toluene to dissolve the precipitated solid was added. The mixture was extracted further with toluene (3×100 ml) and the combined toluene extract was washed with water (3×200 ml). The toluene layers were distilled down to low volume in vacuo and iso-hexane was added (50 ml). The resulting precipitate of the desired product was filtered off, washed with iso-hexane (2×25 ml) and dried in a vacuum oven at 40° C. overnight (6.0 g, 74.4% yield).

1. additionthis was added to the flask
2. additioncontaining the anion of S-1-methoxyproapan-2-ol
3. additionwas added
4. extractionThe mixture was extracted further with toluene (3×100 ml)
5. extractionthe combined toluene extract
6. washwas washed with water (3×200 ml)
7. distillationThe toluene layers were distilled down to low volume in vacuo and iso-hexane
8. additionwas added (50 ml)
9. filtrationThe resulting precipitate of the desired product was filtered off
10. washwashed with iso-hexane (2×25 ml)
11. customdried in a vacuum oven at 40° C. overnight (6.0 g, 74.4% yield)