Abstract: A series of new indolinyl derivatives (Ⅰ_1～5, Ⅱ_1～3 and Ⅲ_1～8) with different substituents at 1-,3-or 5-position were synthesized in order to study the relationship of structure and anticholinesterase activities of CUI XING NING and its derivatives. The method of phase transfer catalysis was successfully applied in the C₃-alkylation of intermediate A as well as in the N-alkylation and the carbamylation. Three by-products were obtained during the C₃-alkylation and their structures and all of the structures of the 24 new compounds (including the intermediats) were identified by spectral and elementary analysis. Preliminary pharmacologic tests showed that most of the compounds have potent anticholinesterase activities. All of the substituents of 1-, 3-or 5-position of the compounds may affect their activities (see Table 4).