반응 #46951

반응 방정식

ethyl acetate

2-(5-iodo-2-isopropyl-4-methoxy-phenoxy)-3-phenylamino-acrylonitrile

guanidine carbonate

DMF

→

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

수율 99.1%

용매

Water

반응 조건

후처리

1. 1
   온도to maintain an internal temperature of 50° C
2. 2
   온도The resulting slurry was cooled to 20° C.
3. 3
   기타Precipitated solids
4. 4
   여과were collected by filtration
5. 5
   세척washed with water (300 ml)
6. 6
   기타dried in a vacuum oven (50° C., 24 inches Hg)

실험 절차

A solution of 2-(5-iodo-2-isopropyl-4-methoxy-phenoxy)-3-phenylamino-acrylonitrile (280 g, 0.64 mol), guanidine carbonate (110 g, 0.61 mol), and 560 ml of DMF was heated to 120° C. for 18 hours. After cooling the mixture to 60° C., 140 ml of ethyl acetate was added. Water (1.12 L) was then added to the mixture at a rate to maintain an internal temperature of 50° C. The resulting slurry was cooled to 20° C. and aged. Precipitated solids were collected by filtration, washed with water (300 ml) followed by isopropanol (500 ml), and dried in a vacuum oven (50° C., 24 inches Hg) to give 242 g of 5-(5-iodo-2-isopropyl-4-methoxy-phenoxy)-pyrimidine-2,4-diamine, 94% yield: m.p. 204.4-205.9 degrees C.; 1HNMR (DMSO) δ=1.2 (d, 6H), 3.3 (m, 1H), 3.8 (s, 3H), 5.85 (s, 2H), 6.4 (s, 2H), 6.9 (d, 2H), 7.35 (s, 1H)

출처