反应详情

温度

30 °C

A stirred mixture of the crude product from step (i) and guanidine carbonate (36.7 g, 0.20 mol) in methanol (389 g) was heated under reflux for 7 hours. The mixture was cooled to 30° C., diluted with water (222 g), and the pH of the solution was adjusted to pH 6.5 with acetic acid. After the mixture was cooled to 5° C., the resulting precipitate was collected by filtration, washed with methanol twice (167 g, 333 g), and dried under reduced pressure to give the subtitle compound as a solid, 32.6 g.

1. temperaturewas heated
2. temperatureunder reflux for 7 hours
3. temperatureAfter the mixture was cooled to 5° C.
4. filtrationthe resulting precipitate was collected by filtration
5. washwashed with methanol twice (167 g, 333 g)
6. customdried under reduced pressure