| 摘要 |
NEW MATERIAL:S-[5-(N-Acetylamino)-2-chlorobenzene]thioacetate expressed by formula I. USE:A synthetic intermediate for a herbicide tetrahydrophthalimide derivative. PREPARATION:4-Chloro-3-chlorosulfonylacetanilide expressed by formula II or 2-chloro-5-nitrobenzenesulfonyl chloride expressed by formula III is reacted with red phosphorus and acetic acid in the presence of an iodine based catalyst, e.g. iodine or sodium iodide, at 50-130 deg.C, preferably 80 deg.C- the boiling point temperature of the acetic acid for 0.5-24hr to afford the aimed compound expressed by formula I. The reaction is carried out using 0.01-0.5 equiv. catalyst, 1.5-3 equiv. red phosphorus and >=1 equiv. acetic acid based on 1 equiv. compound expressed by formula II. If the compound expressed by formula III is used, the reaction is carried out using 0.01-0.5 equiv. catalyst, 2-20 equiv. red phosphorus and >=1 equiv. acetic acid based on 1 equiv. compound expressed by formula I. |
