反应详情

p-Fluoronitrobenzene (14.1 g; 0.1 mole) was dissolved in tetrahydrofuran (100 ml.). Ten percent palladium on charcoal catalyst (0.1 g.) was added to the solution followed by hydrazine (6.0 ml; 0.105 mole), and the resulting mixture stirred at room temperature for about 48 hours with cooling as necessary. The reaction mixture containing N-(4-fluorophenyl) hydroxylamine was dried over anhydrous magnesium sulfate and filtered. To this solution was added methyl isocyanate (6.2 ml; 0.1 mole) and the mixture stirred for about 15 minutes. The reaction mixture was concentrated by distilling and then washed with hexane and filtered to yield 1-methyl-3-(4'-fluorophenyl)-3-hydroxyurea as a yellow solid.

1. temperaturewith cooling as necessary
2. dry with materialwas dried over anhydrous magnesium sulfate
3. filtrationfiltered
4. stirringthe mixture stirred for about 15 minutes
5. concentrationThe reaction mixture was concentrated
6. distillationby distilling
7. washwashed with hexane
8. filtrationfiltered