反应详情

108 ml of absolute n-propanol were added dropwise at room temperature to 1.1 g of sodium hydride (97% strength) in 40 ml of absolute tetrahydrofuran. Stirring was carried out for 30 minutes, after which 7.0 g of 3-[2,4-dichloro-6-fluorobenzothiazol-7-yl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione (compound I.4) were slowly added. Stirring was carried out for 12 hours, after which the solvent was distilled off at reduced pressure and the residue was then taken up in water. 10% strength hydrochloric acid was added to the aqueous phase until the resulting pH was from 3 to 4. The precipitate formed was separated off, washed with water and then dried. Yield: 5.2 g.

1. stirringStirring
2. waitwas carried out for 12 hours
3. distillationafter which the solvent was distilled off at reduced pressure
4. addition10% strength hydrochloric acid was added to the aqueous phase until the resulting pH
5. customThe precipitate formed
6. customwas separated off
7. washwashed with water
8. customdried