反应详情

温度

30 °C

To a mixture of diethyl oxalacetate sodium salt (210 g, 950 mmol) in methanol (500 mL) and water (400 mL) was added 50% aqueous sodium hydroxide (80 g, 1.0 mol) in water (60 mL) over 30 minutes, over which time the temperature remained at 25-30° C. and the pH at 11-12. Then the stirred mixture was heated for an additional 30 min at 30° C. To this mixture was added cyclopropanecarboximidamide monohydrochloride (110 g, 910 mol). The orange solution was heated to 50° C. over 30 minutes and held at that temperature for 5 h. The reaction mixture was cooled to 30° C. and concentrated to half volume at reduced pressure at 35-40° C. and concentrated hydrochloric acid (140 g, 1.4 mol) was added gradually (resulting in foaming) over 30 minutes at 25-30° C. until the pH was about 1-2. The mixture was stirred at 5° C. for 1 h to complete crystallization of the product. After the mixture was cooled to 0° C. the solid was collected by filtration. The solid washed with water (3×60 mL), suction-dried, and then dried in a vacuum-oven at 70° C. to afford the title compound as a beige solid (100 g); m.p. 235-236° C. (dec.).

1. customremained at 25-30° C.
2. temperatureThe orange solution was heated to 50° C. over 30 minutes
3. temperatureThe reaction mixture was cooled to 30° C.
4. concentrationconcentrated to half volume at reduced pressure at 35-40° C.
5. custom(resulting in foaming) over 30 minutes at 25-30° C. until the pH was about 1-2
6. customcrystallization of the product
7. temperatureAfter the mixture was cooled to 0° C. the solid
8. filtrationwas collected by filtration
9. washThe solid washed with water (3×60 mL)
10. customsuction-dried
11. customdried in a vacuum-oven at 70° C.