反应详情

5.00 g (23.3 mmol) of 3-bromobenzoic acid hydrazide are placed in 50 ml tetrahydrofuran at room temperature. 2.70 g (27.2 mmol) of isobutyl isocyanate, dissolved in 10 ml tetrahydrofuran, are rapidly added dropwise with stirring to this suspension. The mixture is firstly further stirred at room temperature and then allowed to stand overnight. The precipitate formed after addition of 100 ml diethyl ether is filtered off and then washed with diethyl ether. An initial quantity of 1.42 g (19% of theory) of the target compound is thus obtained. The mother liquor is concentrated, and the residue again slurried in diethyl ether and filtered. After washing with diethyl ether and drying in vacuo, a further 5.62 g (77% of theory) of the target compound remain.

1. additionare rapidly added dropwise
2. stirringThe mixture is firstly further stirred at room temperature
3. customThe precipitate formed
4. filtrationis filtered off
5. washwashed with diethyl ether
6. customAn initial quantity of 1.42 g (19% of theory) of the target compound is thus obtained
7. concentrationThe mother liquor is concentrated
8. filtrationfiltered
9. washAfter washing with diethyl ether
10. customdrying in vacuo