反应详情

温度

55 °C

Add ethyl 1-[(4-ethoxybenzoyl)amino]cyclopropanecarboxylate (478 g, 1.72 mol) to tetrahydrofuran (2 L) and methanol (1 L). Dissolve lithium hydroxide (LiOH) (144.7 g, 3.45 mol) in water (1 L) and add it to the mixture. Stir the reaction mixture while heating to 55° C. Cool the reaction to ambient temperature and concentrate under reduced pressure. After removing 2.5 L of solvent, dilute the mixture with water (2 L) and immerse it in an ice water bath. Adjust to pH 2 with aqueous 5N hydrochloric acid (750 mL). Filter the precipitate, wash the cake with water (2×2 L), and dry to give the title compound (425 g, 99%) as a white powder: MS (m/z): 250 (M+1).

1. temperatureCool
2. customthe reaction to ambient temperature
3. concentrationconcentrate under reduced pressure
4. customAfter removing 2.5 L of solvent
5. additiondilute the mixture with water (2 L)
6. filtrationFilter the precipitate
7. washwash the cake with water (2×2 L)
8. customdry