Hydrochloric Acid → 4-Methoxy-6-(trifluoromethyl)-1,3,5-triazin-2-amine

Temperature

5 °C

1.8 g of a 30% by weight solution of sodium methanolate in methanol (corresponding to 0.01 mol of sodium methanolate) were added at 22° C. to a solution of 28.8 g (0.1 mol) of 2-amino-4-trichloromethyl-6-trifluoromethyl-1,3,5-triazine in 100 ml of methanol. The pale yellow solution was then refluxed for 30 minutes. The progress of the reaction was followed by thin-layer chromatography on silica gel (mobile phase: diethyl ether/hexane 1:1). After the reaction was complete, 20 ml of water were added, followed by 2 normal hydrochloric acid until the pH was 6-7. After this most of the methanol was removed at 40° C. under reduced pressure, adding 150 ml of water a little at a time so that the product did not agglomerate. To complete precipitation of the product, the resulting mixture was then stirred at 5° C. for 1 hour, after which the product was separated off, washed with a little water and dried at 40° C. under reduced pressure.

1. temperatureThe pale yellow solution was then refluxed for 30 minutes
2. customAfter this most of the methanol was removed at 40° C. under reduced pressure
3. additionadding 150 ml of water a little at a time so that the product
4. customTo complete precipitation of the product
5. customafter which the product was separated off
6. washwashed with a little water
7. customdried at 40° C. under reduced pressure

ORD record

ord-02949f084009433c9fff6abd1f9b68a8

Source dataset

uspto-grants-1992_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05130428