| 摘要 |
<p>2-Benzothiazyl sulphene morpholide is manufactured by treating 2-benzothiazolyl disulphide in an inert organic solvent with at least an equimolecular proportion each of N-chloromorpholine and of morpholine in the presence of an acid acceptor. Preferred solvents are hydrocarbons and halogenated hydrocarbons of the benzene series, whilst the acid acceptor is advantageously an amine, preferably a tertiary amine or excess of morpholine. The N-chloromorpholine may be prepared by chlorinating morpholine in situ in the solvent to be used in the condensation. The acid acceptor may be regenerated for further use by treating it, either in the reaction mixture or after separation and re-slurrying in an anhydrous inert solvent, with ammonia and separating the ammonium chloride formed. When morpholine is used it may be chlorinated before being recycled. In examples (1) 1 mol. of 2-benzothiazolyl disulphide is added to a solution of 1 mol. of N-chloromorpholine and 2 mols. of morpholine in toluene, which is then stirred at 30-45 DEG C., after which the mixture is saturated with anhydrous ammonia, the ammonium chloride formed is filtered off, morpholine is extracted with water and the toluene steam distilled; (2) the toluene in (1) is replaced by chlorobenzene and the proportion of morpholine is increased slightly.</p> |
