反应详情

To a stirred solution of 1.8 g (4.4 mmole) of the product from Example 126 in 50 mL dimethylformamide was added 2.4 g (17.4 mmole) potassium carbonate. The mixture was stirred at room temperature for 1 hour then 1.2 g (5.72 mmole) 2-(chloromethyl)-5-fluorobenzothiazole was added. The mixture was stirred for 18 hours, poured into water, acidified to ph 1-4 with 1N HCl, and extracted with ethyl acetate. The ethyl acetate extract was washed with water and brine and then dried (MgSO4), and concentrated to give a solid. Trituration with ether afforded 2.45 g (97%) of the title product as a solid, mp 218°-220° C. Analysis calculated for C26H18N2S2O5F4 : C, 53.98; H, 3.14; N, 4.84. Found: C, 53.94; H, 2.91; N, 4.55.

1. stirringThe mixture was stirred for 18 hours
2. extractionextracted with ethyl acetate
3. extractionThe ethyl acetate extract
4. washwas washed with water and brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customto give a solid