Reaktion #96269

Reaktionsgleichung

diazabicyclooctane

3,5-dibromo-2,4-dihydroxy-benzaldoxime

methyl isocyanate

→

2,4-Dihydroxy-3,5-dibromo-benzaldoxime tris-(methylcarbamate)

Lösungsmittel

dimethylsulfoxide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwith cooling (<20° C.)
2. 2
   workup.STIRRINGthe mixture was then stirred thoroughly at room temperature for 12 hours
3. 3
   FiltrationThe suspension was filtered with suction
4. 4
   Waschenthe residue was washed with water
5. 5
   workup.DISSOLUTIONdissolved in a little dimethylformamide and active charcoal
6. 6
   workup.ADDITIONwas added to the solution

Vorschrift

6 g of 3,5-dibromo-2,4-dihydroxy-benzaldoxime were dissolved in 50 ml of dimethylsulfoxide and a little diazabicyclooctane was added. 4 ml of methyl isocyanate were now added with cooling (<20° C.) and stirring and the mixture was then stirred thoroughly at room temperature for 12 hours. The reaction mixture was poured into ice-water and salted out. The suspension was filtered with suction, the residue was washed with water and dissolved in a little dimethylformamide and active charcoal was added to the solution.

Quelle