Reaktion #46952

Reaktionsgleichung

5-(5-Iodo-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine

5-(5-iodo-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine

HCl

→

(5-iodo-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine hydrochloride salt

Ausbeute 98.0%

Lösungsmittel

isopropanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe slurry was heated to 75° C. for two hours
2. 2
   TemperaturThe slurry was cooled to 20° C.
3. 3
   SonstigePrecipitated solids
4. 4
   Filtrationwere collected by filtration
5. 5
   Waschenwashed with cold isopropanol
6. 6
   Sonstigedried in a vacuum oven (50° C., 24 inches Hg)

Vorschrift

5-(5-Iodo-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine A mixture of 5-(5-iodo-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine (240 g, 0.60 mol) in 1.2 L of isopropanol was heated to 70° C. An aqueous solution of 6N HCl was added dropwise to the reaction mixture, and the slurry was heated to 75° C. for two hours. The slurry was cooled to 20° C. and aged. Precipitated solids were collected by filtration, washed with cold isopropanol, and dried in a vacuum oven (50° C., 24 inches Hg) to give 232 g of -(5-iodo-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine hydrochloride salt, 98% yield: m.p. 262.0-263.0 degrees C.; 1HNMR (DMSO) δ=1.2 (d, 6H), 3.1 (m, 1H), 3.85 (s, 3H), 6.95 (s, 1H), 7.25 (s, 1H), 7.45 (s, 1H), 7.6 (s, 2H), 8.25 (s, 1H), 8.6 (s, 1H), 11.9 (s, 1H).

Quelle