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ChemicalBook CAS DataBase List 4-(BROMODIFLUOROMETHOXY)NITROBENZENE

4-(BROMODIFLUOROMETHOXY)NITROBENZENE synthesis

5synthesis methods
-

Yield:81932-04-9 50%

Reaction Conditions:

with NaH in N,N-dimethyl-formamide;

Steps:

5.b (b)

(b) Preparation of p-bromodifluoromethoxyphenylisocyanate Into DMF (20 ml.), 50% NaH (5.0 g. 104 m mol) was added and the mixture was cooled on an ice bath. A solution of p-nitrophenol (13.9 g. 100 m mol) in DMF (100 ml.) was added dropwise and the mixture was stirred for 10 minutes. A solution of dibromodifluoromethane (25 g. 119 m mol) in DMF (60 ml.) was added and the mixture was stirred for 5 hours at room temperature. The reaction mixture was poured into water and the product was extracted with ether. The ether layer was dried over anhydrous magnesium sulfate and the solvent was distilled off and the product was distilled to obtain 13.4 g. of p-nitro(bromodifluoromethoxy)benzene (boiling point of 74°-77° C./0.1 mmHg). The yield was 50%.

References:

US4464386,1984,A