反应详情

温度

20 °C

Ethyl benzoylacetate (1,538 g, 8 moles) dissolved in isopropanol (6 l) is placed in a 12 l flask under an atmosphere of nitrogen. Methylhydrazine (410 g, 8.7 moles) in isopropanol (800 ml) is added with stirring in a dropwise manner to the ethyl benzoylacetate solution prewarmed to about 80° C. During the addition external heating is removed. Seeding of the reaction mixture with the product at the point of one-third addition of methylhydrazine causes a copious precipitate of product. This procedure eliminates a large exotherm from occurring at a later stage. After the addition is completed, the reaction mixture is held at about 80° C. for 2 hours. Cooling the slurry to 20° C. and filtering off the solid, a yield of 1,131 g (81%) of product after drying and having a melting point of 211° C. is obtained.

1. customis placed in a 12 l flask under an atmosphere of nitrogen
2. customprewarmed to about 80° C
3. temperatureDuring the addition external heating
4. customis removed
5. additionSeeding of the reaction mixture with the product at the point of one-third addition of methylhydrazine
6. additionAfter the addition
7. filtrationfiltering off the solid
8. dry with materiala yield of 1,131 g (81%) of product after drying
9. customis obtained