تفاعل #1506889

معادلة التفاعل

n-propanol

sodium hydride

3-[2,4-dichloro-6-fluorobenzothiazol-7-yl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

→

3-[4-Chloro-6-fluoro-2-propoxybenzothiazol-7-yl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGStirring
2. 2
   workup.WAITwas carried out for 12 hours
3. 3
   workup.DISTILLATIONafter which the solvent was distilled off at reduced pressure
4. 4
   workup.ADDITION10% strength hydrochloric acid was added to the aqueous phase until the resulting pH
5. 5
   أخرىThe precipitate formed
6. 6
   أخرىwas separated off
7. 7
   غسيلwashed with water
8. 8
   أخرىdried

الإجراء التجريبي

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.

المصدر